Supplementary information (ESI) for Dalton Trans. This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Insertion reactions of ?-diketiminate-stabilised calcium amides with 1,3-dialkylcarbodiimides ; _publ_requested_category FM _publ_contact_author_name 'Michael Hill' _publ_contact_author_email MSH27@BATH.AC.UK loop_ _publ_author_name 'Michael Hill' 'A. Barrett' 'Mark R. Crimmin' 'P. B. Hitchcock' 'P. Procopiou' # Attachment 'msh-oct-2007.cif' data_(3)-may1106 _database_code_depnum_ccdc_archive 'CCDC 667066' _audit_creation_date 2006-05-12T10:44:21-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C45 H59 Ca N3 O' _chemical_formula_sum 'C45 H59 Ca N3 O' _chemical_formula_weight 698.03 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5773(3) _cell_length_b 18.5052(4) _cell_length_c 19.8953(3) _cell_angle_alpha 63.586(1) _cell_angle_beta 79.436(1) _cell_angle_gamma 79.604(1) _cell_volume 4051.04(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28447 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.191 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.409558E-1 _diffrn_orient_matrix_ub_12 0.459955E-1 _diffrn_orient_matrix_ub_13 -0.37613E-1 _diffrn_orient_matrix_ub_21 0.703075E-1 _diffrn_orient_matrix_ub_22 -0.340773E-1 _diffrn_orient_matrix_ub_23 0.154426E-1 _diffrn_orient_matrix_ub_31 0.21251E-2 _diffrn_orient_matrix_ub_32 -0.202566E-1 _diffrn_orient_matrix_ub_33 -0.392451E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_unetI/netI 0.0582 _diffrn_reflns_number 60764 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.4 _diffrn_reflns_theta_max 26 _diffrn_reflns_theta_full 26 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 15835 _reflns_number_gt 10996 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+1.5701P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 15835 _refine_ls_number_parameters 905 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1259 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.457 _refine_diff_density_min -0.27 _refine_diff_density_rms 0.046 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca Ca 0.17863(3) 0.08906(2) 0.76174(2) 0.02448(11) Uani 1 1 d . . . O O 0.10441(12) 0.19490(9) 0.79651(8) 0.0342(4) Uani 1 1 d . . . N1 N 0.34487(13) 0.13898(10) 0.69238(9) 0.0238(4) Uani 1 1 d . . . N2 N 0.12548(13) 0.15162(10) 0.64051(9) 0.0249(4) Uani 1 1 d . . . N3 N 0.12082(14) -0.03793(10) 0.84579(9) 0.0299(4) Uani 1 1 d . . . C1 C 0.35179(16) 0.20381(12) 0.62638(11) 0.0258(5) Uani 1 1 d . . . C2 C 0.26727(17) 0.24071(13) 0.58011(11) 0.0305(5) Uani 1 1 d . . . H2 H 0.279 0.2927 0.5405 0.037 Uiso 1 1 calc R . . C3 C 0.16874(17) 0.21386(12) 0.58251(11) 0.0275(5) Uani 1 1 d . . . C4 C 0.45738(18) 0.24295(14) 0.59414(12) 0.0364(5) Uani 1 1 d . . . H4A H 0.4633 0.2776 0.6185 0.055 Uiso 1 1 calc R . . H4B H 0.4575 0.2759 0.5396 0.055 Uiso 1 1 calc R . . H4C H 0.5193 0.2005 0.6035 0.055 Uiso 1 1 calc R . . C5 C 0.1113(2) 0.25912(15) 0.51191(12) 0.0463(7) Uani 1 1 d . . . H5A H 0.1095 0.2223 0.4889 0.069 Uiso 1 1 calc R . . H5B H 0.1505 0.3051 0.4759 0.069 Uiso 1 1 calc R . . H5C H 0.0367 0.2792 0.5254 0.069 Uiso 1 1 calc R . . C6 C 0.44142(15) 0.10265(12) 0.72965(11) 0.0252(5) Uani 1 1 d . . . C7 C 0.47596(16) 0.13469(12) 0.77352(11) 0.0279(5) Uani 1 1 d . . . C8 C 0.56655(17) 0.09417(14) 0.81190(13) 0.0363(5) Uani 1 1 d . . . H8 H 0.5909 0.1152 0.8414 0.044 Uiso 1 1 calc R . . C9 C 0.62162(18) 0.02449(15) 0.80810(14) 0.0419(6) Uani 1 1 d . . . H9 H 0.6837 -0.0017 0.8342 0.05 Uiso 1 1 calc R . . C10 C 0.58601(18) -0.00694(14) 0.76622(13) 0.0392(6) Uani 1 1 d . . . H10 H 0.6238 -0.0554 0.7643 0.047 Uiso 1 1 calc R . . C11 C 0.49591(16) 0.03050(13) 0.72652(12) 0.0304(5) Uani 1 1 d . . . C12 C 0.41573(18) 0.20945(13) 0.78265(12) 0.0329(5) Uani 1 1 d . . . H12 H 0.3652 0.2374 0.7428 0.039 Uiso 1 1 calc R . . C13 C 0.34692(19) 0.18480(15) 0.85973(13) 0.0411(6) Uani 1 1 d . . . H13A H 0.3086 0.2335 0.8647 0.062 Uiso 1 1 calc R . . H13B H 0.3943 0.1553 0.8999 0.062 Uiso 1 1 calc R . . H13C H 0.2938 0.1498 0.864 0.062 Uiso 1 1 calc R . . C14 C 0.4923(2) 0.26984(14) 0.77243(15) 0.0465(6) Uani 1 1 d . . . H14A H 0.4498 0.3168 0.7787 0.07 Uiso 1 1 calc R . . H14B H 0.5326 0.2879 0.7217 0.07 Uiso 1 1 calc R . . H14C H 0.5436 0.2436 0.8103 0.07 Uiso 1 1 calc R . . C15 C 0.45755(18) -0.00502(14) 0.68067(13) 0.0370(5) Uani 1 1 d . . . H15 H 0.3765 0.007 0.6839 0.044 Uiso 1 1 calc R . . C16 C 0.5017(3) 0.0356(2) 0.59743(16) 0.0681(9) Uani 1 1 d . . . H16A H 0.4749 0.0118 0.5694 0.102 Uiso 1 1 calc R . . H16B H 0.5814 0.0274 0.5922 0.102 Uiso 1 1 calc R . . H16C H 0.4771 0.0939 0.5771 0.102 Uiso 1 1 calc R . . C17 C 0.4838(3) -0.09702(16) 0.71153(18) 0.0649(8) Uani 1 1 d . . . H17A H 0.4568 -0.1164 0.68 0.097 Uiso 1 1 calc R . . H17B H 0.4486 -0.1224 0.7635 0.097 Uiso 1 1 calc R . . H17C H 0.5627 -0.1114 0.711 0.097 Uiso 1 1 calc R . . C18 C 0.03679(16) 0.12069(12) 0.62888(11) 0.0266(5) Uani 1 1 d . . . C19 C -0.07224(17) 0.14674(13) 0.64736(12) 0.0309(5) Uani 1 1 d . . . C20 C -0.15461(18) 0.11086(14) 0.63953(13) 0.0371(6) Uani 1 1 d . . . H20 H -0.2284 0.1276 0.6524 0.045 Uiso 1 1 calc R . . C21 C -0.13077(19) 0.05160(14) 0.61346(13) 0.0390(6) Uani 1 1 d . . . H21 H -0.188 0.0282 0.6078 0.047 Uiso 1 1 calc R . . C22 C -0.02399(19) 0.02600(14) 0.59548(13) 0.0378(5) Uani 1 1 d . . . H22 H -0.0085 -0.0148 0.5773 0.045 Uiso 1 1 calc R . . C23 C 0.06152(17) 0.05889(13) 0.60351(12) 0.0311(5) Uani 1 1 d . . . C24 C -0.10204(18) 0.21090(15) 0.67731(14) 0.0419(6) Uani 1 1 d . . . H24 H -0.0333 0.232 0.6755 0.05 Uiso 1 1 calc R . . C25 C -0.1522(2) 0.1742(2) 0.75945(16) 0.0680(9) Uani 1 1 d . . . H25A H -0.1704 0.2166 0.7778 0.102 Uiso 1 1 calc R . . H25B H -0.1001 0.1314 0.7902 0.102 Uiso 1 1 calc R . . H25C H -0.2185 0.1511 0.7632 0.102 Uiso 1 1 calc R . . C26 C -0.1777(3) 0.28287(18) 0.6283(2) 0.0762(10) Uani 1 1 d . . . H26A H -0.1947 0.3232 0.6492 0.114 Uiso 1 1 calc R . . H26B H -0.2452 0.2637 0.628 0.114 Uiso 1 1 calc R . . H26C H -0.1416 0.3077 0.5766 0.114 Uiso 1 1 calc R . . C27 C 0.17837(19) 0.02620(15) 0.58811(13) 0.0402(6) Uani 1 1 d . . . H27 H 0.2264 0.0578 0.5971 0.048 Uiso 1 1 calc R . . C28 C 0.2076(3) 0.0376(3) 0.50671(19) 0.0982(14) Uani 1 1 d . . . H28A H 0.2837 0.016 0.4993 0.147 Uiso 1 1 calc R . . H28B H 0.1976 0.0955 0.4727 0.147 Uiso 1 1 calc R . . H28C H 0.1603 0.0086 0.4956 0.147 Uiso 1 1 calc R . . C29 C 0.2007(2) -0.06276(18) 0.6435(2) 0.0800(11) Uani 1 1 d . . . H29A H 0.2765 -0.0828 0.6329 0.12 Uiso 1 1 calc R . . H29B H 0.1521 -0.0951 0.6378 0.12 Uiso 1 1 calc R . . H29C H 0.1878 -0.0674 0.6953 0.12 Uiso 1 1 calc R . . C30 C 0.03115(17) -0.08005(12) 0.86348(12) 0.0297(5) Uani 1 1 d . . . C31 C -0.03470(18) -0.06114(14) 0.80683(13) 0.0372(5) Uani 1 1 d . . . H31 H -0.0193 -0.0177 0.7588 0.045 Uiso 1 1 calc R . . C32 C -0.12086(19) -0.10338(15) 0.81858(14) 0.0442(6) Uani 1 1 d . . . H32 H -0.1631 -0.0889 0.7785 0.053 Uiso 1 1 calc R . . C33 C -0.1470(2) -0.16653(15) 0.88762(15) 0.0480(6) Uani 1 1 d . . . H33 H -0.2074 -0.195 0.8959 0.058 Uiso 1 1 calc R . . C34 C -0.0831(2) -0.18725(15) 0.94434(14) 0.0447(6) Uani 1 1 d . . . H34 H -0.0995 -0.2309 0.992 0.054 Uiso 1 1 calc R . . C35 C 0.00453(18) -0.14584(13) 0.93327(12) 0.0365(5) Uani 1 1 d . . . H35 H 0.0475 -0.1619 0.9733 0.044 Uiso 1 1 calc R . . C36 C 0.17676(17) -0.04236(12) 0.90202(11) 0.0295(5) Uani 1 1 d . . . C37 C 0.28924(18) -0.03636(13) 0.88481(13) 0.0351(5) Uani 1 1 d . . . H37 H 0.3255 -0.0385 0.8393 0.042 Uiso 1 1 calc R . . C38 C 0.3490(2) -0.02747(14) 0.93218(15) 0.0496(7) Uani 1 1 d . . . H38 H 0.4247 -0.023 0.9186 0.059 Uiso 1 1 calc R . . C39 C 0.2988(3) -0.02511(16) 0.99880(16) 0.0591(8) Uani 1 1 d . . . H39 H 0.3394 -0.0183 1.031 0.071 Uiso 1 1 calc R . . C40 C 0.1887(3) -0.03279(16) 1.01846(14) 0.0562(7) Uani 1 1 d . . . H40 H 0.154 -0.0319 1.0647 0.067 Uiso 1 1 calc R . . C41 C 0.1288(2) -0.04173(14) 0.97154(12) 0.0397(6) Uani 1 1 d . . . H41 H 0.0535 -0.0476 0.9865 0.048 Uiso 1 1 calc R . . C42 C 0.0449(2) 0.19087(15) 0.86793(13) 0.0421(6) Uani 1 1 d . . . H42A H 0.0943 0.1683 0.9077 0.05 Uiso 1 1 calc R . . H42B H -0.0143 0.1558 0.8842 0.05 Uiso 1 1 calc R . . C43 C -0.0013(3) 0.27686(17) 0.85428(16) 0.0700(9) Uani 1 1 d . . . H43A H -0.0801 0.2797 0.8721 0.084 Uiso 1 1 calc R . . H43B H 0.0362 0.2973 0.8809 0.084 Uiso 1 1 calc R . . C44 C 0.0186(2) 0.32538(16) 0.76997(16) 0.0579(7) Uani 1 1 d . . . H44A H -0.0444 0.3281 0.7451 0.07 Uiso 1 1 calc R . . H44B H 0.0327 0.3812 0.7571 0.07 Uiso 1 1 calc R . . C45 C 0.11662(19) 0.27918(13) 0.74718(13) 0.0401(6) Uani 1 1 d . . . H45A H 0.1195 0.2896 0.6936 0.048 Uiso 1 1 calc R . . H45B H 0.1839 0.2945 0.754 0.048 Uiso 1 1 calc R . . Ca1B Ca 0.63862(3) 0.43139(2) 0.22022(2) 0.02531(11) Uani 1 1 d . A 1 O1B O 0.71730(13) 0.35630(9) 0.15415(8) 0.0398(4) Uani 1 1 d . A 1 N1B N 0.71161(13) 0.34611(10) 0.33661(9) 0.0246(4) Uani 1 1 d . A 1 N2B N 0.48531(13) 0.36402(10) 0.28769(9) 0.0243(4) Uani 1 1 d . A 1 N3B N 0.62617(14) 0.56956(10) 0.13706(9) 0.0299(4) Uani 1 1 d . A 1 C1B C 0.67430(16) 0.27746(12) 0.38773(11) 0.0253(4) Uani 1 1 d . A 1 C2B C 0.57596(16) 0.25072(12) 0.38738(11) 0.0269(5) Uani 1 1 d . A 1 H2B H 0.5691 0.1954 0.4207 0.032 Uiso 1 1 calc R A 1 C3B C 0.48666(16) 0.29153(12) 0.34649(11) 0.0244(4) Uani 1 1 d . A 1 C4B C 0.73593(18) 0.22173(13) 0.45467(12) 0.0347(5) Uani 1 1 d . A 1 H4B1 H 0.801 0.1934 0.4377 0.052 Uiso 1 1 calc R A 1 H4B2 H 0.689 0.1819 0.4927 0.052 Uiso 1 1 calc R A 1 H4B3 H 0.7575 0.2539 0.4769 0.052 Uiso 1 1 calc R A 1 C5B C 0.38447(17) 0.24885(13) 0.37520(12) 0.0347(5) Uani 1 1 d . A 1 H5B1 H 0.3284 0.2792 0.397 0.052 Uiso 1 1 calc R A 1 H5B2 H 0.401 0.1938 0.414 0.052 Uiso 1 1 calc R A 1 H5B3 H 0.3579 0.246 0.3332 0.052 Uiso 1 1 calc R A 1 C6B C 0.80509(16) 0.37159(12) 0.34912(11) 0.0262(5) Uani 1 1 d . A 1 C7B C 0.91231(16) 0.34064(13) 0.33140(11) 0.0301(5) Uani 1 1 d . A 1 C8B C 0.99851(18) 0.37283(14) 0.34010(12) 0.0357(5) Uani 1 1 d . A 1 H8B H 1.0711 0.3534 0.3275 0.043 Uiso 1 1 calc R A 1 C9B C 0.98133(18) 0.43183(14) 0.36638(13) 0.0380(6) Uani 1 1 d . A 1 H9B H 1.0414 0.4518 0.3729 0.046 Uiso 1 1 calc R A 1 C10B C 0.87628(18) 0.46179(14) 0.38316(12) 0.0355(5) Uani 1 1 d . A 1 H10B H 0.8647 0.5026 0.4012 0.043 Uiso 1 1 calc R A 1 C11B C 0.78702(17) 0.43344(13) 0.37423(11) 0.0284(5) Uani 1 1 d . A 1 C12B C 0.93778(18) 0.27566(14) 0.30229(13) 0.0365(5) Uani 1 1 d . A 1 H12B H 0.8682 0.2539 0.307 0.044 Uiso 1 1 calc R A 1 C13B C 0.9842(2) 0.31091(17) 0.21861(14) 0.0493(7) Uani 1 1 d . A 1 H13D H 0.9994 0.2678 0.2012 0.074 Uiso 1 1 calc R A 1 H13E H 1.0517 0.3338 0.2124 0.074 Uiso 1 1 calc R A 1 H13F H 0.9311 0.3537 0.1888 0.074 Uiso 1 1 calc R A 1 C14B C 1.0179(2) 0.20415(15) 0.34832(16) 0.0544(7) Uani 1 1 d . A 1 H14D H 1.0316 0.1635 0.3278 0.082 Uiso 1 1 calc R A 1 H14E H 0.9863 0.1794 0.4013 0.082 Uiso 1 1 calc R A 1 H14F H 1.0865 0.2241 0.3451 0.082 Uiso 1 1 calc R A 1 C15B C 0.67237(18) 0.46925(13) 0.39139(12) 0.0338(5) Uani 1 1 d . A 1 H15B H 0.6261 0.4661 0.3571 0.041 Uiso 1 1 calc R A 1 C16B C 0.6247(2) 0.41928(16) 0.47234(14) 0.0522(7) Uani 1 1 d . A 1 H16D H 0.5508 0.4434 0.4817 0.078 Uiso 1 1 calc R A 1 H16E H 0.6703 0.4188 0.5076 0.078 Uiso 1 1 calc R A 1 H16F H 0.6226 0.3635 0.4797 0.078 Uiso 1 1 calc R A 1 C17B C 0.6649(2) 0.55860(14) 0.37578(14) 0.0438(6) Uani 1 1 d . A 1 H17D H 0.5893 0.5783 0.3875 0.066 Uiso 1 1 calc R A 1 H17E H 0.6896 0.5906 0.3224 0.066 Uiso 1 1 calc R A 1 H17F H 0.7111 0.5642 0.4075 0.066 Uiso 1 1 calc R A 1 C18B C 0.38402(15) 0.40534(12) 0.25888(11) 0.0255(5) Uani 1 1 d . A 1 C19B C 0.35213(17) 0.39932(13) 0.19744(12) 0.0310(5) Uani 1 1 d . A 1 C20B C 0.25982(17) 0.44904(14) 0.16548(13) 0.0372(6) Uani 1 1 d . A 1 H20B H 0.2374 0.4456 0.124 0.045 Uiso 1 1 calc R A 1 C21B C 0.20105(17) 0.50258(14) 0.19252(13) 0.0385(6) Uani 1 1 d . A 1 H21B H 0.1396 0.5365 0.1693 0.046 Uiso 1 1 calc R A 1 C22B C 0.23163(17) 0.50684(13) 0.25345(13) 0.0342(5) Uani 1 1 d . A 1 H22B H 0.1902 0.5436 0.2723 0.041 Uiso 1 1 calc R A 1 C23B C 0.32182(16) 0.45851(12) 0.28818(12) 0.0287(5) Uani 1 1 d . A 1 C24B C 0.41517(19) 0.34351(15) 0.16326(13) 0.0402(6) Uani 1 1 d . A 1 H24B H 0.4764 0.3118 0.1939 0.048 Uiso 1 1 calc R A 1 C25B C 0.4643(2) 0.39307(18) 0.08213(14) 0.0519(7) Uani 1 1 d . A 1 H25D H 0.5052 0.3562 0.0609 0.078 Uiso 1 1 calc R A 1 H25E H 0.5134 0.4285 0.0823 0.078 Uiso 1 1 calc R A 1 H25F H 0.4058 0.4262 0.0514 0.078 Uiso 1 1 calc R A 1 C26B C 0.3446(2) 0.28310(16) 0.16518(15) 0.0516(7) Uani 1 1 d . A 1 H26D H 0.3883 0.248 0.1428 0.077 Uiso 1 1 calc R A 1 H26E H 0.2831 0.3129 0.1363 0.077 Uiso 1 1 calc R A 1 H26F H 0.3172 0.2498 0.2177 0.077 Uiso 1 1 calc R A 1 C27B C 0.35524(18) 0.46867(13) 0.35295(12) 0.0336(5) Uani 1 1 d . A 1 H27B H 0.412 0.423 0.3769 0.04 Uiso 1 1 calc R A 1 C28B C 0.2604(2) 0.46700(16) 0.41388(13) 0.0465(6) Uani 1 1 d . A 1 H28D H 0.2865 0.4736 0.4541 0.07 Uiso 1 1 calc R A 1 H28E H 0.2303 0.415 0.435 0.07 Uiso 1 1 calc R A 1 H28F H 0.2038 0.5114 0.3915 0.07 Uiso 1 1 calc R A 1 C29B C 0.4050(2) 0.54801(15) 0.32235(14) 0.0464(6) Uani 1 1 d . A 1 H29D H 0.427 0.5541 0.3641 0.07 Uiso 1 1 calc R A 1 H29E H 0.3512 0.5935 0.2973 0.07 Uiso 1 1 calc R A 1 H29F H 0.4688 0.5475 0.2859 0.07 Uiso 1 1 calc R A 1 C30B C 0.54961(17) 0.63129(13) 0.09707(11) 0.0293(5) Uani 1 1 d . A 1 C31B C 0.44085(18) 0.61659(14) 0.11229(12) 0.0374(6) Uani 1 1 d . A 1 H31B H 0.4226 0.5635 0.1454 0.045 Uiso 1 1 calc R A 1 C32B C 0.3588(2) 0.67743(15) 0.08044(14) 0.0477(7) Uani 1 1 d . A 1 H32B H 0.2854 0.6657 0.0931 0.057 Uiso 1 1 calc R A 1 C33B C 0.3822(2) 0.75471(15) 0.03076(15) 0.0505(7) Uani 1 1 d . A 1 H33B H 0.3258 0.7962 0.0088 0.061 Uiso 1 1 calc R A 1 C34B C 0.4891(2) 0.77035(14) 0.01359(13) 0.0437(6) Uani 1 1 d . A 1 H34B H 0.5065 0.8232 -0.0212 0.052 Uiso 1 1 calc R A 1 C35B C 0.57190(19) 0.71058(13) 0.04605(12) 0.0341(5) Uani 1 1 d . A 1 H35B H 0.6449 0.7233 0.0337 0.041 Uiso 1 1 calc R A 1 C36B C 0.73622(17) 0.57267(12) 0.11157(11) 0.0285(5) Uani 1 1 d . A 1 C37B C 0.81018(18) 0.53798(13) 0.16565(12) 0.0356(5) Uani 1 1 d . A 1 H37B H 0.7829 0.521 0.2175 0.043 Uiso 1 1 calc R A 1 C38B C 0.92136(19) 0.52763(15) 0.14610(14) 0.0437(6) Uani 1 1 d . A 1 H38B H 0.9684 0.5025 0.1846 0.052 Uiso 1 1 calc R A 1 C39B C 0.9645(2) 0.55332(15) 0.07152(14) 0.0471(7) Uani 1 1 d . A 1 H39B H 1.0408 0.5463 0.058 0.056 Uiso 1 1 calc R A 1 C40B C 0.89379(19) 0.58975(14) 0.01628(13) 0.0418(6) Uani 1 1 d . A 1 H40B H 0.9226 0.6083 -0.0355 0.05 Uiso 1 1 calc R A 1 C41B C 0.78289(18) 0.59948(13) 0.03507(12) 0.0345(5) Uani 1 1 d . A 1 H41B H 0.7367 0.6246 -0.0039 0.041 Uiso 1 1 calc R A 1 C42B C 0.7687(2) 0.38458(15) 0.07595(13) 0.0463(6) Uani 1 1 d . A 1 H42C H 0.8276 0.4177 0.0675 0.056 Uiso 1 1 calc R A 1 H42D H 0.7145 0.4179 0.0404 0.056 Uiso 1 1 calc R A 1 C43B C 0.8136(2) 0.30966(17) 0.06485(16) 0.0594(8) Uani 1 1 d . A 1 H43C H 0.8909 0.294 0.0743 0.071 Uiso 1 1 calc R A 1 H43D H 0.8078 0.3178 0.0129 0.071 Uiso 1 1 calc R A 1 C44B C 0.7428(3) 0.24594(17) 0.12278(17) 0.0615(8) Uani 1 1 d . A 1 H44C H 0.6739 0.2493 0.1037 0.074 Uiso 1 1 calc R A 1 H44D H 0.7814 0.1905 0.1369 0.074 Uiso 1 1 calc R A 1 C45B C 0.7229(2) 0.26813(14) 0.18717(14) 0.0458(6) Uani 1 1 d . A 1 H45C H 0.6537 0.2498 0.2185 0.055 Uiso 1 1 calc R A 1 H45D H 0.7829 0.2429 0.2193 0.055 Uiso 1 1 calc R A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca 0.0248(2) 0.0240(2) 0.0223(2) -0.00737(18) -0.00178(16) -0.00464(17) O 0.0420(9) 0.0286(8) 0.0286(8) -0.0120(7) 0.0040(7) -0.0048(7) N1 0.0241(9) 0.0232(9) 0.0241(9) -0.0093(7) -0.0039(7) -0.0041(7) N2 0.0255(9) 0.0234(9) 0.0240(9) -0.0074(7) -0.0053(7) -0.0034(7) N3 0.0327(10) 0.0269(10) 0.0262(9) -0.0070(8) -0.0017(8) -0.0076(8) C1 0.0274(11) 0.0261(11) 0.0243(11) -0.0108(9) -0.0002(8) -0.0063(9) C2 0.0371(12) 0.0247(11) 0.0246(11) -0.0035(9) -0.0039(9) -0.0100(9) C3 0.0313(12) 0.0256(11) 0.0246(11) -0.0094(9) -0.0058(9) -0.0017(9) C4 0.0339(13) 0.0383(13) 0.0321(12) -0.0085(10) 0.0002(10) -0.0138(10) C5 0.0494(15) 0.0483(15) 0.0309(13) 0.0008(11) -0.0150(11) -0.0178(12) C6 0.0211(10) 0.0255(11) 0.0257(11) -0.0079(9) -0.0001(8) -0.0059(8) C7 0.0251(11) 0.0285(11) 0.0278(11) -0.0092(9) -0.0010(9) -0.0068(9) C8 0.0297(12) 0.0422(14) 0.0401(13) -0.0172(11) -0.0089(10) -0.0071(10) C9 0.0288(12) 0.0445(15) 0.0520(15) -0.0198(12) -0.0150(11) 0.0051(11) C10 0.0287(12) 0.0376(13) 0.0525(15) -0.0231(12) -0.0072(11) 0.0067(10) C11 0.0245(11) 0.0326(12) 0.0328(12) -0.0137(10) 0.0004(9) -0.0045(9) C12 0.0360(13) 0.0310(12) 0.0358(12) -0.0153(10) -0.0122(10) -0.0031(10) C13 0.0434(14) 0.0407(14) 0.0440(14) -0.0228(12) -0.0063(11) -0.0025(11) C14 0.0554(16) 0.0352(14) 0.0538(16) -0.0178(12) -0.0137(12) -0.0128(12) C15 0.0306(12) 0.0373(13) 0.0493(14) -0.0251(12) -0.0062(10) 0.0011(10) C16 0.085(2) 0.081(2) 0.0536(18) -0.0430(17) 0.0080(16) -0.0235(18) C17 0.077(2) 0.0460(17) 0.088(2) -0.0405(16) -0.0294(17) 0.0056(15) C18 0.0277(11) 0.0250(11) 0.0230(10) -0.0039(9) -0.0081(8) -0.0045(9) C19 0.0275(12) 0.0307(12) 0.0305(12) -0.0077(10) -0.0087(9) -0.0021(9) C20 0.0281(12) 0.0407(14) 0.0392(13) -0.0124(11) -0.0096(10) -0.0023(10) C21 0.0347(13) 0.0409(14) 0.0450(14) -0.0158(12) -0.0156(11) -0.0087(11) C22 0.0435(14) 0.0354(13) 0.0427(14) -0.0213(11) -0.0125(11) -0.0040(11) C23 0.0323(12) 0.0316(12) 0.0300(12) -0.0121(10) -0.0091(9) -0.0020(9) C24 0.0279(12) 0.0456(15) 0.0589(16) -0.0293(13) -0.0040(11) -0.0022(10) C25 0.0594(19) 0.101(3) 0.0663(19) -0.0565(19) 0.0211(15) -0.0358(17) C26 0.063(2) 0.059(2) 0.115(3) -0.050(2) -0.0274(19) 0.0247(16) C27 0.0364(13) 0.0467(15) 0.0517(15) -0.0333(13) -0.0103(11) -0.0001(11) C28 0.051(2) 0.187(4) 0.080(2) -0.088(3) -0.0036(17) 0.013(2) C29 0.0494(18) 0.0509(18) 0.132(3) -0.035(2) -0.0212(19) 0.0137(14) C30 0.0285(12) 0.0238(11) 0.0344(12) -0.0123(10) 0.0003(9) -0.0012(9) C31 0.0371(13) 0.0321(13) 0.0362(13) -0.0078(10) -0.0063(10) -0.0052(10) C32 0.0342(13) 0.0446(15) 0.0530(15) -0.0185(13) -0.0085(11) -0.0056(11) C33 0.0390(14) 0.0487(16) 0.0585(17) -0.0231(14) 0.0014(12) -0.0170(12) C34 0.0499(15) 0.0379(14) 0.0416(14) -0.0115(11) 0.0065(12) -0.0198(12) C35 0.0407(13) 0.0329(13) 0.0320(12) -0.0096(10) -0.0018(10) -0.0082(10) C36 0.0321(12) 0.0195(11) 0.0285(11) -0.0032(9) -0.0020(9) -0.0036(9) C37 0.0338(13) 0.0258(12) 0.0341(12) -0.0030(10) -0.0033(10) -0.0023(9) C38 0.0476(15) 0.0347(14) 0.0520(17) 0.0028(12) -0.0217(13) -0.0112(11) C39 0.089(2) 0.0404(15) 0.0442(16) -0.0004(13) -0.0331(16) -0.0208(15) C40 0.087(2) 0.0473(16) 0.0351(14) -0.0138(12) -0.0050(14) -0.0213(15) C41 0.0478(15) 0.0354(13) 0.0331(13) -0.0129(11) 0.0009(11) -0.0081(11) C42 0.0472(15) 0.0441(15) 0.0320(13) -0.0178(11) 0.0088(11) -0.0071(11) C43 0.096(2) 0.0512(18) 0.0509(17) -0.0255(15) 0.0087(16) 0.0124(16) C44 0.0676(19) 0.0363(15) 0.0600(18) -0.0181(13) -0.0013(14) 0.0052(13) C45 0.0433(14) 0.0311(13) 0.0401(14) -0.0104(11) -0.0010(11) -0.0065(10) Ca1B 0.0238(2) 0.0255(2) 0.0231(2) -0.00624(18) -0.00414(16) -0.00394(17) O1B 0.0474(10) 0.0334(9) 0.0368(9) -0.0166(7) 0.0057(7) -0.0069(7) N1B 0.0227(9) 0.0254(9) 0.0242(9) -0.0087(7) -0.0042(7) -0.0027(7) N2B 0.0215(9) 0.0251(9) 0.0261(9) -0.0099(8) -0.0052(7) -0.0023(7) N3B 0.0290(10) 0.0296(10) 0.0264(9) -0.0067(8) -0.0049(7) -0.0044(8) C1B 0.0268(11) 0.0236(11) 0.0247(11) -0.0100(9) -0.0044(8) -0.0004(8) C2B 0.0296(11) 0.0213(11) 0.0267(11) -0.0067(9) -0.0035(9) -0.0048(9) C3B 0.0264(11) 0.0253(11) 0.0237(10) -0.0128(9) -0.0010(8) -0.0042(8) C4B 0.0351(13) 0.0309(12) 0.0300(12) -0.0034(10) -0.0095(10) -0.0040(10) C5B 0.0309(12) 0.0352(13) 0.0343(12) -0.0099(10) -0.0006(10) -0.0115(10) C6B 0.0254(11) 0.0285(11) 0.0196(10) -0.0030(9) -0.0076(8) -0.0054(9) C7B 0.0266(11) 0.0308(12) 0.0269(11) -0.0054(9) -0.0068(9) -0.0034(9) C8B 0.0252(12) 0.0395(13) 0.0345(12) -0.0071(11) -0.0077(9) -0.0039(10) C9B 0.0322(13) 0.0418(14) 0.0387(13) -0.0100(11) -0.0117(10) -0.0130(10) C10B 0.0399(14) 0.0369(13) 0.0316(12) -0.0121(10) -0.0076(10) -0.0119(10) C11B 0.0313(12) 0.0303(12) 0.0206(10) -0.0060(9) -0.0052(9) -0.0068(9) C12B 0.0258(12) 0.0384(13) 0.0448(14) -0.0169(11) -0.0072(10) -0.0015(10) C13B 0.0426(15) 0.0566(17) 0.0511(16) -0.0274(14) -0.0029(12) -0.0017(12) C14B 0.0402(15) 0.0404(15) 0.0730(19) -0.0163(14) -0.0160(13) 0.0069(11) C15B 0.0353(13) 0.0379(13) 0.0335(12) -0.0184(11) -0.0045(10) -0.0075(10) C16B 0.0563(17) 0.0423(15) 0.0531(16) -0.0222(13) 0.0133(13) -0.0092(12) C17B 0.0452(15) 0.0366(14) 0.0510(15) -0.0183(12) -0.0101(12) -0.0040(11) C18B 0.0196(10) 0.0266(11) 0.0288(11) -0.0086(9) -0.0032(8) -0.0069(8) C19B 0.0274(11) 0.0334(12) 0.0325(12) -0.0123(10) -0.0061(9) -0.0061(9) C20B 0.0309(12) 0.0448(14) 0.0382(13) -0.0157(11) -0.0148(10) -0.0044(10) C21B 0.0218(11) 0.0408(14) 0.0474(14) -0.0120(12) -0.0118(10) -0.0008(10) C22B 0.0247(11) 0.0349(13) 0.0440(13) -0.0177(11) -0.0049(10) -0.0020(9) C23B 0.0246(11) 0.0278(11) 0.0344(12) -0.0128(10) -0.0034(9) -0.0064(9) C24B 0.0399(14) 0.0470(15) 0.0398(13) -0.0233(12) -0.0166(11) 0.0053(11) C25B 0.0431(15) 0.0737(19) 0.0478(15) -0.0350(15) -0.0048(12) -0.0036(13) C26B 0.0710(19) 0.0449(15) 0.0467(15) -0.0228(13) -0.0204(13) -0.0024(13) C27B 0.0322(12) 0.0323(12) 0.0401(13) -0.0189(11) -0.0068(10) -0.0005(9) C28B 0.0522(16) 0.0490(16) 0.0398(14) -0.0183(12) 0.0008(12) -0.0171(12) C29B 0.0443(15) 0.0522(16) 0.0525(15) -0.0291(13) 0.0011(12) -0.0179(12) C30B 0.0359(12) 0.0278(11) 0.0252(11) -0.0112(9) -0.0085(9) -0.0013(9) C31B 0.0369(13) 0.0307(12) 0.0362(13) -0.0056(10) -0.0067(10) -0.0042(10) C32B 0.0350(14) 0.0443(15) 0.0530(16) -0.0111(13) -0.0099(12) 0.0006(11) C33B 0.0504(16) 0.0363(14) 0.0553(16) -0.0102(13) -0.0206(13) 0.0075(12) C34B 0.0566(17) 0.0269(12) 0.0426(14) -0.0086(11) -0.0133(12) -0.0020(11) C35B 0.0410(13) 0.0285(12) 0.0330(12) -0.0119(10) -0.0066(10) -0.0051(10) C36B 0.0349(12) 0.0223(11) 0.0266(11) -0.0062(9) -0.0067(9) -0.0073(9) C37B 0.0367(13) 0.0371(13) 0.0296(12) -0.0060(10) -0.0082(10) -0.0138(10) C38B 0.0362(14) 0.0420(14) 0.0444(15) -0.0052(12) -0.0133(11) -0.0109(11) C39B 0.0306(13) 0.0469(15) 0.0537(16) -0.0113(13) -0.0023(12) -0.0106(11) C40B 0.0400(14) 0.0421(14) 0.0359(13) -0.0102(11) 0.0038(11) -0.0126(11) C41B 0.0390(13) 0.0330(12) 0.0276(12) -0.0079(10) -0.0061(10) -0.0060(10) C42B 0.0490(15) 0.0473(15) 0.0347(13) -0.0140(12) 0.0071(11) -0.0084(12) C43B 0.0641(19) 0.0617(19) 0.0597(18) -0.0380(15) 0.0120(14) -0.0112(15) C44B 0.070(2) 0.0509(17) 0.072(2) -0.0360(16) -0.0001(15) -0.0074(15) C45B 0.0541(16) 0.0334(14) 0.0465(15) -0.0141(12) -0.0044(12) -0.0059(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca N2 2.3306(16) . ? Ca O 2.3441(15) . ? Ca N3 2.3499(16) . ? Ca N1 2.3736(16) . ? Ca C36 2.7680(19) . ? Ca C37 2.889(2) . ? O C45 1.445(3) . ? O C42 1.456(3) . ? N1 C1 1.329(2) . ? N1 C6 1.438(2) . ? N2 C3 1.330(2) . ? N2 C18 1.438(2) . ? N3 C30 1.390(3) . ? N3 C36 1.393(3) . ? C1 C2 1.408(3) . ? C1 C4 1.523(3) . ? C2 C3 1.402(3) . ? C2 H2 0.95 . ? C3 C5 1.518(3) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C11 1.409(3) . ? C6 C7 1.412(3) . ? C7 C8 1.395(3) . ? C7 C12 1.522(3) . ? C8 C9 1.376(3) . ? C8 H8 0.95 . ? C9 C10 1.377(3) . ? C9 H9 0.95 . ? C10 C11 1.395(3) . ? C10 H10 0.95 . ? C11 C15 1.519(3) . ? C12 C14 1.527(3) . ? C12 C13 1.530(3) . ? C12 H12 1 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C16 1.524(3) . ? C15 C17 1.525(3) . ? C15 H15 1 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C19 1.408(3) . ? C18 C23 1.410(3) . ? C19 C20 1.392(3) . ? C19 C24 1.514(3) . ? C20 C21 1.375(3) . ? C20 H20 0.95 . ? C21 C22 1.379(3) . ? C21 H21 0.95 . ? C22 C23 1.392(3) . ? C22 H22 0.95 . ? C23 C27 1.516(3) . ? C24 C25 1.523(4) . ? C24 C26 1.535(4) . ? C24 H24 1 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C28 1.519(4) . ? C27 C29 1.528(4) . ? C27 H27 1 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 C31 1.402(3) . ? C30 C35 1.412(3) . ? C31 C32 1.375(3) . ? C31 H31 0.95 . ? C32 C33 1.380(3) . ? C32 H32 0.95 . ? C33 C34 1.380(3) . ? C33 H33 0.95 . ? C34 C35 1.384(3) . ? C34 H34 0.95 . ? C35 H35 0.95 . ? C36 C37 1.406(3) . ? C36 C41 1.408(3) . ? C37 C38 1.386(3) . ? C37 H37 0.95 . ? C38 C39 1.375(4) . ? C38 H38 0.95 . ? C39 C40 1.383(4) . ? C39 H39 0.95 . ? C40 C41 1.381(4) . ? C40 H40 0.95 . ? C41 H41 0.95 . ? C42 C43 1.511(4) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? C43 C44 1.507(4) . ? C43 H43A 0.99 . ? C43 H43B 0.99 . ? C44 C45 1.489(3) . ? C44 H44A 0.99 . ? C44 H44B 0.99 . ? C45 H45A 0.99 . ? C45 H45B 0.99 . ? Ca1B O1B 2.3000(16) . ? Ca1B N3B 2.3423(17) . ? Ca1B N2B 2.3460(16) . ? Ca1B N1B 2.3876(16) . ? Ca1B C36B 2.859(2) . ? Ca1B C37B 2.915(2) . ? O1B C45B 1.456(3) . ? O1B C42B 1.463(3) . ? N1B C1B 1.326(2) . ? N1B C6B 1.442(2) . ? N2B C3B 1.331(2) . ? N2B C18B 1.436(2) . ? N3B C36B 1.386(3) . ? N3B C30B 1.393(3) . ? C1B C2B 1.415(3) . ? C1B C4B 1.519(3) . ? C2B C3B 1.406(3) . ? C2B H2B 0.95 . ? C3B C5B 1.516(3) . ? C4B H4B1 0.98 . ? C4B H4B2 0.98 . ? C4B H4B3 0.98 . ? C5B H5B1 0.98 . ? C5B H5B2 0.98 . ? C5B H5B3 0.98 . ? C6B C11B 1.409(3) . ? C6B C7B 1.413(3) . ? C7B C8B 1.398(3) . ? C7B C12B 1.516(3) . ? C8B C9B 1.376(3) . ? C8B H8B 0.95 . ? C9B C10B 1.380(3) . ? C9B H9B 0.95 . ? C10B C11B 1.391(3) . ? C10B H10B 0.95 . ? C11B C15B 1.520(3) . ? C12B C13B 1.534(3) . ? C12B C14B 1.544(3) . ? C12B H12B 1 . ? C13B H13D 0.98 . ? C13B H13E 0.98 . ? C13B H13F 0.98 . ? C14B H14D 0.98 . ? C14B H14E 0.98 . ? C14B H14F 0.98 . ? C15B C16B 1.526(3) . ? C15B C17B 1.529(3) . ? C15B H15B 1 . ? C16B H16D 0.98 . ? C16B H16E 0.98 . ? C16B H16F 0.98 . ? C17B H17D 0.98 . ? C17B H17E 0.98 . ? C17B H17F 0.98 . ? C18B C19B 1.409(3) . ? C18B C23B 1.409(3) . ? C19B C20B 1.401(3) . ? C19B C24B 1.513(3) . ? C20B C21B 1.372(3) . ? C20B H20B 0.95 . ? C21B C22B 1.375(3) . ? C21B H21B 0.95 . ? C22B C23B 1.391(3) . ? C22B H22B 0.95 . ? C23B C27B 1.522(3) . ? C24B C26B 1.532(3) . ? C24B C25B 1.533(3) . ? C24B H24B 1 . ? C25B H25D 0.98 . ? C25B H25E 0.98 . ? C25B H25F 0.98 . ? C26B H26D 0.98 . ? C26B H26E 0.98 . ? C26B H26F 0.98 . ? C27B C29B 1.521(3) . ? C27B C28B 1.530(3) . ? C27B H27B 1 . ? C28B H28D 0.98 . ? C28B H28E 0.98 . ? C28B H28F 0.98 . ? C29B H29D 0.98 . ? C29B H29E 0.98 . ? C29B H29F 0.98 . ? C30B C31B 1.395(3) . ? C30B C35B 1.407(3) . ? C31B C32B 1.385(3) . ? C31B H31B 0.95 . ? C32B C33B 1.377(3) . ? C32B H32B 0.95 . ? C33B C34B 1.376(3) . ? C33B H33B 0.95 . ? C34B C35B 1.386(3) . ? C34B H34B 0.95 . ? C35B H35B 0.95 . ? C36B C37B 1.404(3) . ? C36B C41B 1.419(3) . ? C37B C38B 1.383(3) . ? C37B H37B 0.95 . ? C38B C39B 1.375(3) . ? C38B H38B 0.95 . ? C39B C40B 1.391(3) . ? C39B H39B 0.95 . ? C40B C41B 1.377(3) . ? C40B H40B 0.95 . ? C41B H41B 0.95 . ? C42B C43B 1.495(4) . ? C42B H42C 0.99 . ? C42B H42D 0.99 . ? C43B C44B 1.518(4) . ? C43B H43C 0.99 . ? C43B H43D 0.99 . ? C44B C45B 1.478(4) . ? C44B H44C 0.99 . ? C44B H44D 0.99 . ? C45B H45C 0.99 . ? C45B H45D 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ca O 96.57(6) . . ? N2 Ca N3 118.78(6) . . ? O Ca N3 114.37(6) . . ? N2 Ca N1 80.97(6) . . ? O Ca N1 99.63(6) . . ? N3 Ca N1 136.59(6) . . ? N2 Ca C36 148.96(6) . . ? O Ca C36 100.72(6) . . ? N3 Ca C36 30.19(6) . . ? N1 Ca C36 120.69(6) . . ? N2 Ca C37 155.28(7) . . ? O Ca C37 107.99(6) . . ? N3 Ca C37 53.21(6) . . ? N1 Ca C37 92.01(6) . . ? C36 Ca C37 28.68(6) . . ? C45 O C42 107.86(17) . . ? C45 O Ca 122.82(13) . . ? C42 O Ca 129.27(13) . . ? C1 N1 C6 118.59(16) . . ? C1 N1 Ca 124.10(13) . . ? C6 N1 Ca 116.77(11) . . ? C3 N2 C18 118.04(16) . . ? C3 N2 Ca 125.48(13) . . ? C18 N2 Ca 116.47(11) . . ? C30 N3 C36 121.27(17) . . ? C30 N3 Ca 139.43(13) . . ? C36 N3 Ca 91.76(11) . . ? N1 C1 C2 124.79(18) . . ? N1 C1 C4 120.60(17) . . ? C2 C1 C4 114.59(17) . . ? C3 C2 C1 131.01(18) . . ? C3 C2 H2 114.5 . . ? C1 C2 H2 114.5 . . ? N2 C3 C2 124.73(18) . . ? N2 C3 C5 119.29(18) . . ? C2 C3 C5 115.96(18) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 120.50(18) . . ? C11 C6 N1 118.45(18) . . ? C7 C6 N1 120.85(18) . . ? C8 C7 C6 118.3(2) . . ? C8 C7 C12 119.14(19) . . ? C6 C7 C12 122.52(18) . . ? C9 C8 C7 121.7(2) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C10 119.5(2) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C9 C10 C11 121.8(2) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C10 C11 C6 118.3(2) . . ? C10 C11 C15 121.1(2) . . ? C6 C11 C15 120.62(18) . . ? C7 C12 C14 112.60(19) . . ? C7 C12 C13 110.47(18) . . ? C14 C12 C13 110.08(19) . . ? C7 C12 H12 107.8 . . ? C14 C12 H12 107.8 . . ? C13 C12 H12 107.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 111.5(2) . . ? C11 C15 C17 113.2(2) . . ? C16 C15 C17 110.6(2) . . ? C11 C15 H15 107 . . ? C16 C15 H15 107 . . ? C17 C15 H15 107 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 120.28(19) . . ? C19 C18 N2 121.34(19) . . ? C23 C18 N2 118.23(18) . . ? C19 C18 Ca 109.61(13) . . ? C23 C18 Ca 112.39(13) . . ? C20 C19 C18 118.8(2) . . ? C20 C19 C24 119.3(2) . . ? C18 C19 C24 121.88(19) . . ? C21 C20 C19 121.0(2) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 120.2(2) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 121.1(2) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 118.6(2) . . ? C22 C23 C27 120.3(2) . . ? C18 C23 C27 121.12(19) . . ? C19 C24 C25 110.8(2) . . ? C19 C24 C26 111.8(2) . . ? C25 C24 C26 111.1(2) . . ? C19 C24 H24 107.7 . . ? C25 C24 H24 107.7 . . ? C26 C24 H24 107.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C28 112.3(2) . . ? C23 C27 C29 110.5(2) . . ? C28 C27 C29 111.4(3) . . ? C23 C27 H27 107.5 . . ? C28 C27 H27 107.5 . . ? C29 C27 H27 107.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 C31 118.68(18) . . ? N3 C30 C35 125.13(19) . . ? C31 C30 C35 116.0(2) . . ? C32 C31 C30 122.2(2) . . ? C32 C31 H31 118.9 . . ? C30 C31 H31 118.9 . . ? C31 C32 C33 121.1(2) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C34 C33 C32 118.2(2) . . ? C34 C33 H33 120.9 . . ? C32 C33 H33 120.9 . . ? C33 C34 C35 121.5(2) . . ? C33 C34 H34 119.3 . . ? C35 C34 H34 119.3 . . ? C34 C35 C30 121.1(2) . . ? C34 C35 H35 119.5 . . ? C30 C35 H35 119.5 . . ? N3 C36 C37 117.70(19) . . ? N3 C36 C41 125.7(2) . . ? C37 C36 C41 116.1(2) . . ? N3 C36 Ca 58.05(9) . . ? C37 C36 Ca 80.43(12) . . ? C41 C36 Ca 126.43(15) . . ? C38 C37 C36 122.0(2) . . ? C38 C37 Ca 128.28(16) . . ? C36 C37 Ca 70.89(11) . . ? C38 C37 H37 119 . . ? C36 C37 H37 119 . . ? Ca C37 H37 72.5 . . ? C39 C38 C37 120.2(2) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 119.4(2) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? C41 C40 C39 120.7(3) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C40 C41 C36 121.5(2) . . ? C40 C41 H41 119.2 . . ? C36 C41 H41 119.2 . . ? O C42 C43 106.48(19) . . ? O C42 H42A 110.4 . . ? C43 C42 H42A 110.4 . . ? O C42 H42B 110.4 . . ? C43 C42 H42B 110.4 . . ? H42A C42 H42B 108.6 . . ? C44 C43 C42 104.9(2) . . ? C44 C43 H43A 110.8 . . ? C42 C43 H43A 110.8 . . ? C44 C43 H43B 110.8 . . ? C42 C43 H43B 110.8 . . ? H43A C43 H43B 108.8 . . ? C45 C44 C43 103.4(2) . . ? C45 C44 H44A 111.1 . . ? C43 C44 H44A 111.1 . . ? C45 C44 H44B 111.1 . . ? C43 C44 H44B 111.1 . . ? H44A C44 H44B 109 . . ? O C45 C44 104.86(18) . . ? O C45 H45A 110.8 . . ? C44 C45 H45A 110.8 . . ? O C45 H45B 110.8 . . ? C44 C45 H45B 110.8 . . ? H45A C45 H45B 108.9 . . ? O1B Ca1B N3B 109.20(6) . . ? O1B Ca1B N2B 101.46(6) . . ? N3B Ca1B N2B 122.72(6) . . ? O1B Ca1B N1B 98.00(6) . . ? N3B Ca1B N1B 137.02(6) . . ? N2B Ca1B N1B 81.49(5) . . ? O1B Ca1B C36B 92.59(6) . . ? N3B Ca1B C36B 28.79(6) . . ? N2B Ca1B C36B 151.39(6) . . ? N1B Ca1B C36B 121.37(6) . . ? O1B Ca1B C37B 94.84(6) . . ? N3B Ca1B C37B 52.76(6) . . ? N2B Ca1B C37B 163.42(7) . . ? N1B Ca1B C37B 93.35(6) . . ? C36B Ca1B C37B 28.13(6) . . ? C45B O1B C42B 108.44(17) . . ? C45B O1B Ca1B 122.80(13) . . ? C42B O1B Ca1B 128.76(13) . . ? C1B N1B C6B 119.33(16) . . ? C1B N1B Ca1B 124.67(13) . . ? C6B N1B Ca1B 115.96(11) . . ? C3B N2B C18B 119.53(16) . . ? C3B N2B Ca1B 125.52(13) . . ? C18B N2B Ca1B 114.89(11) . . ? C36B N3B C30B 120.46(16) . . ? C36B N3B Ca1B 96.75(12) . . ? C30B N3B Ca1B 139.49(13) . . ? N1B C1B C2B 125.04(17) . . ? N1B C1B C4B 120.47(17) . . ? C2B C1B C4B 114.46(17) . . ? C3B C2B C1B 131.41(18) . . ? C3B C2B H2B 114.3 . . ? C1B C2B H2B 114.3 . . ? N2B C3B C2B 125.06(18) . . ? N2B C3B C5B 119.36(17) . . ? C2B C3B C5B 115.55(17) . . ? C11B C6B C7B 120.30(18) . . ? C11B C6B N1B 117.87(18) . . ? C7B C6B N1B 121.65(19) . . ? C8B C7B C6B 118.0(2) . . ? C8B C7B C12B 118.82(19) . . ? C6B C7B C12B 123.15(19) . . ? C9B C8B C7B 121.9(2) . . ? C9B C8B H8B 119 . . ? C7B C8B H8B 119 . . ? C8B C9B C10B 119.5(2) . . ? C8B C9B H9B 120.2 . . ? C10B C9B H9B 120.2 . . ? C9B C10B C11B 121.3(2) . . ? C9B C10B H10B 119.3 . . ? C11B C10B H10B 119.3 . . ? C10B C11B C6B 118.9(2) . . ? C10B C11B C15B 120.0(2) . . ? C6B C11B C15B 121.11(18) . . ? C7B C12B C13B 111.20(19) . . ? C7B C12B C14B 112.25(19) . . ? C13B C12B C14B 109.3(2) . . ? C7B C12B H12B 108 . . ? C13B C12B H12B 108 . . ? C14B C12B H12B 108 . . ? C12B C13B H13D 109.5 . . ? C12B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C12B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C12B C14B H14D 109.5 . . ? C12B C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C12B C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C11B C15B C16B 111.24(18) . . ? C11B C15B C17B 113.29(18) . . ? C16B C15B C17B 110.5(2) . . ? C11B C15B H15B 107.2 . . ? C16B C15B H15B 107.2 . . ? C17B C15B H15B 107.2 . . ? C15B C16B H16D 109.5 . . ? C15B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C15B C17B H17D 109.5 . . ? C15B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C15B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C19B C18B C23B 120.10(18) . . ? C19B C18B N2B 120.83(19) . . ? C23B C18B N2B 118.78(17) . . ? C19B C18B Ca1B 107.71(13) . . ? C23B C18B Ca1B 112.48(12) . . ? C20B C19B C18B 118.3(2) . . ? C20B C19B C24B 118.89(19) . . ? C18B C19B C24B 122.80(18) . . ? C21B C20B C19B 121.7(2) . . ? C21B C20B H20B 119.2 . . ? C19B C20B H20B 119.2 . . ? C20B C21B C22B 119.6(2) . . ? C20B C21B H21B 120.2 . . ? C22B C21B H21B 120.2 . . ? C21B C22B C23B 121.5(2) . . ? C21B C22B H22B 119.2 . . ? C23B C22B H22B 119.2 . . ? C22B C23B C18B 118.80(19) . . ? C22B C23B C27B 119.3(2) . . ? C18B C23B C27B 121.76(18) . . ? C19B C24B C26B 112.0(2) . . ? C19B C24B C25B 110.4(2) . . ? C26B C24B C25B 110.5(2) . . ? C19B C24B H24B 107.9 . . ? C26B C24B H24B 107.9 . . ? C25B C24B H24B 107.9 . . ? C24B C25B H25D 109.5 . . ? C24B C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C24B C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C24B C26B H26D 109.5 . . ? C24B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C24B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C29B C27B C23B 109.65(18) . . ? C29B C27B C28B 109.49(19) . . ? C23B C27B C28B 112.94(18) . . ? C29B C27B H27B 108.2 . . ? C23B C27B H27B 108.2 . . ? C28B C27B H27B 108.2 . . ? C27B C28B H28D 109.5 . . ? C27B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C27B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? N3B C30B C31B 118.49(18) . . ? N3B C30B C35B 124.83(19) . . ? C31B C30B C35B 116.48(19) . . ? C32B C31B C30B 121.7(2) . . ? C32B C31B H31B 119.1 . . ? C30B C31B H31B 119.1 . . ? C33B C32B C31B 121.0(2) . . ? C33B C32B H32B 119.5 . . ? C31B C32B H32B 119.5 . . ? C34B C33B C32B 118.4(2) . . ? C34B C33B H33B 120.8 . . ? C32B C33B H33B 120.8 . . ? C33B C34B C35B 121.3(2) . . ? C33B C34B H34B 119.3 . . ? C35B C34B H34B 119.3 . . ? C34B C35B C30B 121.1(2) . . ? C34B C35B H35B 119.5 . . ? C30B C35B H35B 119.5 . . ? N3B C36B C37B 117.97(18) . . ? N3B C36B C41B 125.83(18) . . ? C37B C36B C41B 115.8(2) . . ? N3B C36B Ca1B 54.46(9) . . ? C37B C36B Ca1B 78.16(12) . . ? C41B C36B Ca1B 135.10(15) . . ? C38B C37B C36B 122.4(2) . . ? C38B C37B Ca1B 134.06(17) . . ? C36B C37B Ca1B 73.71(11) . . ? C38B C37B H37B 118.8 . . ? C36B C37B H37B 118.8 . . ? Ca1B C37B H37B 64.5 . . ? C39B C38B C37B 120.7(2) . . ? C39B C38B H38B 119.7 . . ? C37B C38B H38B 119.7 . . ? C38B C39B C40B 118.5(2) . . ? C38B C39B H39B 120.7 . . ? C40B C39B H39B 120.7 . . ? C41B C40B C39B 121.3(2) . . ? C41B C40B H40B 119.3 . . ? C39B C40B H40B 119.3 . . ? C40B C41B C36B 121.3(2) . . ? C40B C41B H41B 119.4 . . ? C36B C41B H41B 119.4 . . ? O1B C42B C43B 105.82(19) . . ? O1B C42B H42C 110.6 . . ? C43B C42B H42C 110.6 . . ? O1B C42B H42D 110.6 . . ? C43B C42B H42D 110.6 . . ? H42C C42B H42D 108.7 . . ? C42B C43B C44B 103.7(2) . . ? C42B C43B H43C 111 . . ? C44B C43B H43C 111 . . ? C42B C43B H43D 111 . . ? C44B C43B H43D 111 . . ? H43C C43B H43D 109 . . ? C45B C44B C43B 102.3(2) . . ? C45B C44B H44C 111.3 . . ? C43B C44B H44C 111.3 . . ? C45B C44B H44D 111.3 . . ? C43B C44B H44D 111.3 . . ? H44C C44B H44D 109.2 . . ? O1B C45B C44B 105.9(2) . . ? O1B C45B H45C 110.6 . . ? C44B C45B H45C 110.6 . . ? O1B C45B H45D 110.6 . . ? C44B C45B H45D 110.6 . . ? H45C C45B H45D 108.7 . . ? #===END data_(6)-oct1406 _database_code_depnum_ccdc_archive 'CCDC 667067' _audit_creation_date 2006-10-23T10:44:56-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C58 H89 Ca N5 O' _chemical_formula_sum 'C58 H89 Ca N5 O' _chemical_formula_weight 912.42 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.1755(3) _cell_length_b 11.3831(2) _cell_length_c 21.1589(3) _cell_angle_alpha 90 _cell_angle_beta 113.849(1) _cell_angle_gamma 90 _cell_volume 5545.87(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 49901 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.155 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9101 _exptl_absorpt_correction_T_max 0.9589 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.448604E-1 _diffrn_orient_matrix_ub_12 -0.71763E-2 _diffrn_orient_matrix_ub_13 -0.42004E-2 _diffrn_orient_matrix_ub_21 0.25207E-1 _diffrn_orient_matrix_ub_22 -0.36246E-2 _diffrn_orient_matrix_ub_23 0.432017E-1 _diffrn_orient_matrix_ub_31 -0.47244E-2 _diffrn_orient_matrix_ub_32 -0.874809E-1 _diffrn_orient_matrix_ub_33 -0.14454E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_unetI/netI 0.029 _diffrn_reflns_number 70644 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 10880 _reflns_number_gt 8688 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H atom on N3 was refined; other H atoms were in riding mode. The C53 cyclohexyl group is disordered over two resolved conformations which were restrained to be equivalent using the SAME instruction and included with isotropic C atoms. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+3.6166P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 10880 _refine_ls_number_parameters 595 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1348 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.407 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.042 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca Ca 0.227651(14) 0.51007(3) 0.250433(17) 0.02398(10) Uani 1 1 d . A . O O 0.19627(6) 0.68710(12) 0.28788(8) 0.0432(4) Uani 1 1 d . . . N1 N 0.17551(6) 0.54347(14) 0.12915(8) 0.0291(3) Uani 1 1 d . . . N2 N 0.13682(6) 0.42347(14) 0.23478(8) 0.0297(3) Uani 1 1 d . . . N3 N 0.40533(6) 0.42080(14) 0.33364(8) 0.0286(3) Uani 1 1 d . . . H3X H 0.4254(10) 0.484(2) 0.3394(11) 0.039(6) Uiso 1 1 d . . . N4 N 0.32734(6) 0.54742(13) 0.32213(8) 0.0308(3) Uani 1 1 d . . . N5 N 0.30389(6) 0.36471(13) 0.27712(8) 0.0296(3) Uani 1 1 d . . . C1 C 0.15241(8) 0.44441(18) 0.09702(9) 0.0329(4) Uani 1 1 d . . . C2 C 0.13291(9) 0.35093(19) 0.12582(10) 0.0384(5) Uani 1 1 d . . . H2 H 0.1275 0.2791 0.1011 0.046 Uiso 1 1 calc R . . C3 C 0.11999(8) 0.34460(18) 0.18459(10) 0.0347(4) Uani 1 1 d . . . C4 C 0.14566(10) 0.4226(2) 0.02326(11) 0.0519(6) Uani 1 1 d . . . H4A H 0.1794 0.3788 0.0238 0.078 Uiso 1 1 calc R . . H4B H 0.143 0.498 -0.0002 0.078 Uiso 1 1 calc R . . H4C H 0.1103 0.377 -0.0014 0.078 Uiso 1 1 calc R . . C5 C 0.08408(11) 0.2392(2) 0.18752(13) 0.0542(6) Uani 1 1 d . . . H5A H 0.043 0.2616 0.1701 0.081 Uiso 1 1 calc R . . H5B H 0.0971 0.2123 0.2354 0.081 Uiso 1 1 calc R . . H5C H 0.0889 0.1758 0.159 0.081 Uiso 1 1 calc R . . C6 C 0.18398(8) 0.63945(17) 0.09032(9) 0.0308(4) Uani 1 1 d . . . C7 C 0.14041(9) 0.7260(2) 0.06427(11) 0.0443(5) Uani 1 1 d . . . C8 C 0.14959(11) 0.8216(2) 0.02872(12) 0.0541(6) Uani 1 1 d . . . H8 H 0.1201 0.8794 0.0103 0.065 Uiso 1 1 calc R . . C9 C 0.20051(11) 0.8338(2) 0.01970(12) 0.0521(6) Uani 1 1 d . . . H9 H 0.206 0.8995 -0.0047 0.063 Uiso 1 1 calc R . . C10 C 0.24315(10) 0.75075(19) 0.04620(11) 0.0424(5) Uani 1 1 d . . . H10 H 0.2783 0.7601 0.0402 0.051 Uiso 1 1 calc R . . C11 C 0.23627(8) 0.65276(17) 0.08167(9) 0.0312(4) Uani 1 1 d . . . C12 C 0.08413(11) 0.7168(3) 0.07469(16) 0.0690(8) Uani 1 1 d . . . H12 H 0.093 0.6726 0.1186 0.083 Uiso 1 1 calc R . . C13 C 0.06079(16) 0.8383(3) 0.0830(2) 0.1068(15) Uani 1 1 d . . . H13A H 0.0452 0.8787 0.0383 0.16 Uiso 1 1 calc R . . H13B H 0.0924 0.885 0.1165 0.16 Uiso 1 1 calc R . . H13C H 0.0299 0.8285 0.0996 0.16 Uiso 1 1 calc R . . C14 C 0.03875(13) 0.6478(5) 0.0174(2) 0.1208(16) Uani 1 1 d . . . H14A H 0.0314 0.6851 -0.0271 0.181 Uiso 1 1 calc R . . H14B H 0.0027 0.6461 0.0247 0.181 Uiso 1 1 calc R . . H14C H 0.0526 0.5673 0.0174 0.181 Uiso 1 1 calc R . . C15 C 0.28523(8) 0.56424(19) 0.10981(11) 0.0367(5) Uani 1 1 d . . . H15 H 0.273 0.5017 0.1344 0.044 Uiso 1 1 calc R . . C16 C 0.29793(11) 0.5053(2) 0.05247(14) 0.0571(6) Uani 1 1 d . . . H16A H 0.3111 0.5645 0.0284 0.086 Uiso 1 1 calc R . . H16B H 0.2625 0.4676 0.0196 0.086 Uiso 1 1 calc R . . H16C H 0.3283 0.4459 0.0727 0.086 Uiso 1 1 calc R . . C17 C 0.34032(10) 0.6204(3) 0.16175(13) 0.0592(7) Uani 1 1 d . . . H17A H 0.3319 0.6593 0.198 0.089 Uiso 1 1 calc R . . H17B H 0.3547 0.6785 0.1383 0.089 Uiso 1 1 calc R . . H17C H 0.3699 0.5597 0.1825 0.089 Uiso 1 1 calc R . . C18 C 0.11195(8) 0.42437(17) 0.28479(10) 0.0311(4) Uani 1 1 d . . . C19 C 0.05750(8) 0.47780(19) 0.26895(11) 0.0386(5) Uani 1 1 d . . . C20 C 0.03746(9) 0.4891(2) 0.32121(12) 0.0446(5) Uani 1 1 d . . . H20 H 0.0009 0.5253 0.311 0.053 Uiso 1 1 calc R . . C21 C 0.06922(9) 0.4491(2) 0.38706(12) 0.0445(5) Uani 1 1 d . . . H21 H 0.0549 0.4584 0.422 0.053 Uiso 1 1 calc R . . C22 C 0.12211(9) 0.3952(2) 0.40217(11) 0.0403(5) Uani 1 1 d . . . H22 H 0.1438 0.3669 0.4476 0.048 Uiso 1 1 calc R . . C23 C 0.14419(8) 0.38160(17) 0.35171(10) 0.0342(4) Uani 1 1 d . . . C24 C 0.02040(9) 0.5246(2) 0.19720(13) 0.0523(6) Uani 1 1 d . . . H24 H 0.0403 0.5053 0.166 0.063 Uiso 1 1 calc R . . C25 C 0.01343(14) 0.6577(3) 0.19773(18) 0.0804(9) Uani 1 1 d . . . H25A H 0.0517 0.6951 0.2131 0.121 Uiso 1 1 calc R . . H25B H -0.0047 0.6786 0.2294 0.121 Uiso 1 1 calc R . . H25C H -0.0111 0.6848 0.151 0.121 Uiso 1 1 calc R . . C26 C -0.03964(12) 0.4659(4) 0.16794(17) 0.0914(11) Uani 1 1 d . . . H26A H -0.0615 0.4923 0.1203 0.137 Uiso 1 1 calc R . . H26B H -0.0608 0.4874 0.1963 0.137 Uiso 1 1 calc R . . H26C H -0.035 0.3803 0.1685 0.137 Uiso 1 1 calc R . . C27 C 0.20204(9) 0.32091(19) 0.37066(11) 0.0402(5) Uani 1 1 d . . . H27 H 0.2118 0.3252 0.3293 0.048 Uiso 1 1 calc R . . C28 C 0.25012(11) 0.3831(3) 0.42925(19) 0.0818(10) Uani 1 1 d . . . H28A H 0.2876 0.3476 0.4363 0.123 Uiso 1 1 calc R . . H28B H 0.2435 0.3755 0.4717 0.123 Uiso 1 1 calc R . . H28C H 0.2504 0.4664 0.4178 0.123 Uiso 1 1 calc R . . C29 C 0.19906(14) 0.1922(2) 0.38671(17) 0.0717(8) Uani 1 1 d . . . H29A H 0.1909 0.1846 0.4281 0.108 Uiso 1 1 calc R . . H29B H 0.2363 0.1545 0.3949 0.108 Uiso 1 1 calc R . . H29C H 0.1681 0.1542 0.3475 0.108 Uiso 1 1 calc R . . C30 C 0.43780(7) 0.31429(15) 0.35362(9) 0.0268(4) Uani 1 1 d . . . C31 C 0.43525(7) 0.24539(16) 0.40768(9) 0.0287(4) Uani 1 1 d . . . C32 C 0.46557(8) 0.13975(17) 0.42298(10) 0.0339(4) Uani 1 1 d . . . H32 H 0.463 0.0903 0.4578 0.041 Uiso 1 1 calc R . . C33 C 0.49937(8) 0.10522(17) 0.38858(10) 0.0368(5) Uani 1 1 d . . . H33 H 0.5191 0.032 0.3992 0.044 Uiso 1 1 calc R . . C34 C 0.50437(8) 0.17737(18) 0.33877(10) 0.0355(4) Uani 1 1 d . . . H34 H 0.5291 0.1547 0.3168 0.043 Uiso 1 1 calc R . . C35 C 0.47389(8) 0.28262(17) 0.32021(9) 0.0306(4) Uani 1 1 d . . . C36 C 0.40318(8) 0.28848(18) 0.45069(10) 0.0357(4) Uani 1 1 d . . . H36 H 0.3673 0.3301 0.419 0.043 Uiso 1 1 calc R . . C37 C 0.38458(11) 0.1899(2) 0.48631(14) 0.0564(6) Uani 1 1 d . . . H37A H 0.3617 0.2229 0.5101 0.085 Uiso 1 1 calc R . . H37B H 0.4191 0.1508 0.52 0.085 Uiso 1 1 calc R . . H37C H 0.361 0.1328 0.4517 0.085 Uiso 1 1 calc R . . C38 C 0.44068(11) 0.3772(2) 0.50476(12) 0.0533(6) Uani 1 1 d . . . H38A H 0.4521 0.4409 0.4817 0.08 Uiso 1 1 calc R . . H38B H 0.4755 0.3378 0.5377 0.08 Uiso 1 1 calc R . . H38C H 0.4184 0.4096 0.5294 0.08 Uiso 1 1 calc R . . C39 C 0.48192(9) 0.36227(19) 0.26700(11) 0.0406(5) Uani 1 1 d . . . H39 H 0.4485 0.4182 0.2496 0.049 Uiso 1 1 calc R . . C40 C 0.48282(18) 0.2945(3) 0.20522(16) 0.0870(10) Uani 1 1 d . . . H40A H 0.4479 0.2455 0.1854 0.13 Uiso 1 1 calc R . . H40B H 0.5174 0.2445 0.2203 0.13 Uiso 1 1 calc R . . H40C H 0.4837 0.3501 0.1703 0.13 Uiso 1 1 calc R . . C41 C 0.53703(13) 0.4334(3) 0.30067(18) 0.0836(10) Uani 1 1 d . . . H41A H 0.5705 0.3802 0.319 0.125 Uiso 1 1 calc R . . H41B H 0.5349 0.4801 0.3385 0.125 Uiso 1 1 calc R . . H41C H 0.5414 0.4858 0.2664 0.125 Uiso 1 1 calc R . . C42 C 0.19586(14) 0.7962(2) 0.25439(16) 0.0657(7) Uani 1 1 d . . . H42A H 0.1689 0.792 0.2051 0.079 Uiso 1 1 calc R . . H42B H 0.2352 0.8144 0.2572 0.079 Uiso 1 1 calc R . . C43 C 0.1767(2) 0.8880(3) 0.2900(2) 0.0957(12) Uani 1 1 d . . . H43A H 0.1354 0.9083 0.263 0.115 Uiso 1 1 calc R . . H43B H 0.2005 0.9599 0.2965 0.115 Uiso 1 1 calc R . . C44 C 0.18493(13) 0.8361(2) 0.35788(15) 0.0683(8) Uani 1 1 d . . . H44A H 0.1552 0.8654 0.3735 0.082 Uiso 1 1 calc R . . H44B H 0.224 0.8544 0.3936 0.082 Uiso 1 1 calc R . . C45 C 0.17812(11) 0.7070(2) 0.34338(13) 0.0533(6) Uani 1 1 d . . . H45A H 0.2027 0.6617 0.3849 0.064 Uiso 1 1 calc R . . H45B H 0.1371 0.683 0.3295 0.064 Uiso 1 1 calc R . . C46 C 0.34526(7) 0.44163(15) 0.31132(9) 0.0257(4) Uani 1 1 d . A . C47 C 0.36620(8) 0.62956(16) 0.37265(10) 0.0323(4) Uani 1 1 d . . . H47 H 0.4056 0.5928 0.3939 0.039 Uiso 1 1 calc R . . C48 C 0.37146(12) 0.7435(2) 0.33885(12) 0.0568(7) Uani 1 1 d . . . H48A H 0.332 0.7745 0.3115 0.068 Uiso 1 1 calc R . . H48B H 0.3901 0.7273 0.3065 0.068 Uiso 1 1 calc R . . C49 C 0.40678(13) 0.8373(2) 0.39070(13) 0.0622(7) Uani 1 1 d . . . H49A H 0.4479 0.8123 0.413 0.075 Uiso 1 1 calc R . . H49B H 0.4052 0.9119 0.366 0.075 Uiso 1 1 calc R . . C50 C 0.38342(10) 0.8571(2) 0.44553(14) 0.0560(7) Uani 1 1 d . . . H50A H 0.4081 0.9151 0.4797 0.067 Uiso 1 1 calc R . . H50B H 0.3435 0.8891 0.4239 0.067 Uiso 1 1 calc R . . C51 C 0.38283(10) 0.7433(2) 0.48164(12) 0.0494(6) Uani 1 1 d . . . H51A H 0.3671 0.7571 0.517 0.059 Uiso 1 1 calc R . . H51B H 0.423 0.7134 0.5054 0.059 Uiso 1 1 calc R . . C52 C 0.34556(9) 0.6519(2) 0.42964(11) 0.0439(5) Uani 1 1 d . . . H52A H 0.3466 0.5773 0.4541 0.053 Uiso 1 1 calc R . . H52B H 0.3048 0.6794 0.4089 0.053 Uiso 1 1 calc R . . C53 C 0.31556(8) 0.25432(17) 0.25016(9) 0.0308(4) Uiso 0.62 1 d PD A 1 H53 H 0.3535 0.2221 0.2836 0.037 Uiso 0.62 1 calc PR A 1 C54 C 0.26650(16) 0.1658(3) 0.2428(2) 0.0450(8) Uiso 0.62 1 d PD A 1 H54A H 0.2662 0.1517 0.2888 0.054 Uiso 0.62 1 calc PR A 1 H54B H 0.2286 0.2002 0.2127 0.054 Uiso 0.62 1 calc PR A 1 C55 C 0.27452(19) 0.0475(4) 0.2119(2) 0.0568(10) Uiso 0.62 1 d PD A 1 H55A H 0.3091 0.0066 0.2455 0.068 Uiso 0.62 1 calc PR A 1 H55B H 0.2402 -0.003 0.203 0.068 Uiso 0.62 1 calc PR A 1 C56 C 0.28190(18) 0.0661(4) 0.1455(2) 0.0548(10) Uiso 0.62 1 d PD A 1 H56A H 0.291 -0.0101 0.1298 0.066 Uiso 0.62 1 calc PR A 1 H56B H 0.2447 0.0945 0.1098 0.066 Uiso 0.62 1 calc PR A 1 C57 C 0.32879(19) 0.1522(4) 0.1522(2) 0.0541(10) Uiso 0.62 1 d PD A 1 H57A H 0.3295 0.1656 0.1063 0.065 Uiso 0.62 1 calc PR A 1 H57B H 0.3669 0.1199 0.1833 0.065 Uiso 0.62 1 calc PR A 1 C58 C 0.31801(16) 0.2687(3) 0.18121(17) 0.0395(7) Uiso 0.62 1 d PD A 1 H58A H 0.3495 0.3245 0.1855 0.047 Uiso 0.62 1 calc PR A 1 H58B H 0.2809 0.3027 0.1484 0.047 Uiso 0.62 1 calc PR A 1 C53A C 0.31556(8) 0.25432(17) 0.25016(9) 0.0308(4) Uiso 0.38 1 d PD A 2 H53A H 0.3583 0.2491 0.2631 0.037 Uiso 0.38 1 calc PR A 2 C54A C 0.2985(3) 0.1540(5) 0.2803(3) 0.0403(12) Uiso 0.38 1 d PD A 2 H54C H 0.2565 0.1598 0.2697 0.048 Uiso 0.38 1 calc PR A 2 H54D H 0.3199 0.1566 0.3312 0.048 Uiso 0.38 1 calc PR A 2 C55A C 0.3103(3) 0.0371(6) 0.2538(3) 0.0548(16) Uiso 0.38 1 d PD A 2 H55C H 0.3526 0.0284 0.2669 0.066 Uiso 0.38 1 calc PR A 2 H55D H 0.2975 -0.0277 0.2755 0.066 Uiso 0.38 1 calc PR A 2 C56A C 0.2795(3) 0.0293(7) 0.1780(4) 0.0619(18) Uiso 0.38 1 d PD A 2 H56C H 0.2371 0.0299 0.1654 0.074 Uiso 0.38 1 calc PR A 2 H56D H 0.2894 -0.046 0.162 0.074 Uiso 0.38 1 calc PR A 2 C57A C 0.2950(4) 0.1302(7) 0.1414(4) 0.068(2) Uiso 0.38 1 d PD A 2 H57C H 0.2709 0.1259 0.0911 0.082 Uiso 0.38 1 calc PR A 2 H57D H 0.3363 0.1241 0.1487 0.082 Uiso 0.38 1 calc PR A 2 C58A C 0.2844(3) 0.2484(6) 0.1701(3) 0.0507(15) Uiso 0.38 1 d PD A 2 H58C H 0.2422 0.2596 0.156 0.061 Uiso 0.38 1 calc PR A 2 H58D H 0.2987 0.3132 0.1498 0.061 Uiso 0.38 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca 0.02181(17) 0.02595(19) 0.02438(18) -0.00070(14) 0.00954(14) -0.00098(14) O 0.0481(8) 0.0337(8) 0.0516(9) -0.0052(7) 0.0242(7) 0.0044(6) N1 0.0243(7) 0.0379(9) 0.0269(8) 0.0020(7) 0.0120(6) 0.0010(6) N2 0.0268(8) 0.0340(9) 0.0321(8) -0.0006(7) 0.0157(6) -0.0037(6) N3 0.0241(7) 0.0210(8) 0.0396(9) 0.0008(7) 0.0117(7) -0.0001(6) N4 0.0235(7) 0.0242(8) 0.0401(9) -0.0089(7) 0.0082(7) -0.0004(6) N5 0.0266(7) 0.0253(8) 0.0336(8) -0.0063(6) 0.0089(6) -0.0012(6) C1 0.0263(9) 0.0467(12) 0.0276(9) -0.0035(8) 0.0128(8) -0.0018(8) C2 0.0400(11) 0.0413(12) 0.0390(11) -0.0101(9) 0.0212(9) -0.0100(9) C3 0.0304(9) 0.0375(11) 0.0397(11) -0.0029(9) 0.0178(8) -0.0064(8) C4 0.0518(13) 0.0753(17) 0.0328(11) -0.0130(11) 0.0214(10) -0.0196(12) C5 0.0652(15) 0.0518(14) 0.0587(15) -0.0148(12) 0.0385(13) -0.0267(12) C6 0.0329(9) 0.0368(10) 0.0231(9) 0.0026(8) 0.0117(7) 0.0023(8) C7 0.0413(11) 0.0543(14) 0.0394(11) 0.0121(10) 0.0186(9) 0.0158(10) C8 0.0626(15) 0.0536(15) 0.0487(13) 0.0217(11) 0.0252(12) 0.0263(12) C9 0.0750(16) 0.0417(13) 0.0478(13) 0.0174(10) 0.0332(12) 0.0091(12) C10 0.0500(12) 0.0435(12) 0.0420(11) 0.0061(10) 0.0271(10) -0.0012(10) C11 0.0347(10) 0.0348(10) 0.0268(9) 0.0005(8) 0.0152(8) 0.0000(8) C12 0.0451(14) 0.089(2) 0.0813(19) 0.0347(16) 0.0342(14) 0.0325(14) C13 0.102(3) 0.122(3) 0.133(3) 0.067(3) 0.085(2) 0.077(2) C14 0.0394(16) 0.177(5) 0.136(3) 0.006(3) 0.025(2) 0.004(2) C15 0.0353(10) 0.0413(11) 0.0425(11) 0.0099(9) 0.0249(9) 0.0031(9) C16 0.0593(15) 0.0562(15) 0.0697(17) -0.0019(13) 0.0404(13) 0.0100(12) C17 0.0390(12) 0.0824(19) 0.0502(14) 0.0067(13) 0.0119(11) 0.0021(12) C18 0.0305(9) 0.0317(10) 0.0372(10) -0.0045(8) 0.0201(8) -0.0079(8) C19 0.0303(10) 0.0462(12) 0.0444(12) -0.0043(9) 0.0203(9) -0.0048(9) C20 0.0311(10) 0.0567(14) 0.0532(13) -0.0100(11) 0.0247(10) -0.0050(9) C21 0.0421(12) 0.0581(14) 0.0463(12) -0.0155(11) 0.0312(10) -0.0159(10) C22 0.0413(11) 0.0490(13) 0.0372(11) -0.0043(9) 0.0226(9) -0.0100(9) C23 0.0368(10) 0.0339(10) 0.0397(11) -0.0007(8) 0.0235(9) -0.0069(8) C24 0.0356(11) 0.0748(17) 0.0517(14) 0.0081(12) 0.0230(10) 0.0113(11) C25 0.082(2) 0.081(2) 0.091(2) 0.0260(18) 0.0487(18) 0.0297(17) C26 0.0469(15) 0.144(3) 0.0653(19) 0.017(2) 0.0044(14) -0.0087(18) C27 0.0473(12) 0.0426(12) 0.0406(11) 0.0118(9) 0.0280(10) 0.0084(9) C28 0.0357(13) 0.083(2) 0.115(3) -0.0241(19) 0.0185(15) 0.0045(13) C29 0.085(2) 0.0470(15) 0.097(2) 0.0171(15) 0.0515(18) 0.0142(14) C30 0.0219(8) 0.0252(9) 0.0295(9) -0.0038(7) 0.0063(7) -0.0005(7) C31 0.0231(8) 0.0285(9) 0.0308(9) -0.0018(7) 0.0071(7) -0.0016(7) C32 0.0329(10) 0.0288(10) 0.0344(10) 0.0019(8) 0.0078(8) 0.0000(8) C33 0.0344(10) 0.0273(10) 0.0408(11) -0.0038(8) 0.0071(9) 0.0073(8) C34 0.0307(9) 0.0367(11) 0.0380(10) -0.0064(9) 0.0128(8) 0.0064(8) C35 0.0267(9) 0.0325(10) 0.0314(9) -0.0021(8) 0.0104(8) 0.0017(7) C36 0.0345(10) 0.0382(11) 0.0364(10) 0.0068(9) 0.0164(8) 0.0074(8) C37 0.0607(15) 0.0592(16) 0.0637(15) 0.0213(13) 0.0401(13) 0.0129(12) C38 0.0599(14) 0.0542(15) 0.0474(13) -0.0109(11) 0.0235(11) 0.0073(12) C39 0.0395(11) 0.0454(12) 0.0421(11) 0.0073(9) 0.0219(9) 0.0098(9) C40 0.147(3) 0.075(2) 0.0691(19) 0.0048(16) 0.076(2) 0.003(2) C41 0.0710(19) 0.076(2) 0.091(2) 0.0333(18) 0.0198(17) -0.0228(16) C42 0.0855(19) 0.0390(14) 0.0837(19) 0.0034(13) 0.0457(16) 0.0090(13) C43 0.157(4) 0.0432(16) 0.116(3) -0.0022(17) 0.086(3) 0.0212(19) C44 0.0719(18) 0.0595(17) 0.0698(18) -0.0217(14) 0.0248(15) 0.0134(14) C45 0.0550(14) 0.0543(15) 0.0572(14) -0.0101(12) 0.0295(12) 0.0046(11) C46 0.0245(8) 0.0262(9) 0.0263(9) 0.0019(7) 0.0103(7) 0.0006(7) C47 0.0226(8) 0.0291(10) 0.0418(11) -0.0093(8) 0.0097(8) -0.0020(7) C48 0.0754(17) 0.0421(13) 0.0472(13) -0.0109(11) 0.0191(12) -0.0282(12) C49 0.0839(18) 0.0376(13) 0.0526(14) -0.0069(11) 0.0149(13) -0.0275(13) C50 0.0448(12) 0.0360(12) 0.0673(16) -0.0236(11) 0.0022(11) 0.0023(10) C51 0.0422(12) 0.0600(15) 0.0472(13) -0.0244(11) 0.0193(10) -0.0131(11) C52 0.0403(11) 0.0486(13) 0.0437(12) -0.0141(10) 0.0178(10) -0.0141(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca N2 2.3870(15) . ? Ca N4 2.3879(15) . ? Ca N1 2.3936(15) . ? Ca O 2.4123(14) . ? Ca N5 2.4215(15) . ? O C42 1.428(3) . ? O C45 1.440(3) . ? N1 C1 1.324(3) . ? N1 C6 1.434(2) . ? N2 C3 1.323(2) . ? N2 C18 1.431(2) . ? N3 C46 1.410(2) . ? N3 C30 1.427(2) . ? N3 H3X 0.86(2) . ? N4 C46 1.338(2) . ? N4 C47 1.459(2) . ? N5 C46 1.329(2) . ? N5 C53 1.458(2) . ? C1 C2 1.409(3) . ? C1 C4 1.520(3) . ? C2 C3 1.409(3) . ? C2 H2 0.95 . ? C3 C5 1.518(3) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C11 1.409(3) . ? C6 C7 1.410(3) . ? C7 C8 1.394(3) . ? C7 C12 1.523(3) . ? C8 C9 1.377(3) . ? C8 H8 0.95 . ? C9 C10 1.369(3) . ? C9 H9 0.95 . ? C10 C11 1.394(3) . ? C10 H10 0.95 . ? C11 C15 1.515(3) . ? C12 C14 1.507(5) . ? C12 C13 1.540(4) . ? C12 H12 1 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C17 1.519(3) . ? C15 C16 1.529(3) . ? C15 H15 1 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C23 1.404(3) . ? C18 C19 1.411(3) . ? C19 C20 1.394(3) . ? C19 C24 1.521(3) . ? C20 C21 1.374(3) . ? C20 H20 0.95 . ? C21 C22 1.381(3) . ? C21 H21 0.95 . ? C22 C23 1.397(3) . ? C22 H22 0.95 . ? C23 C27 1.512(3) . ? C24 C25 1.526(4) . ? C24 C26 1.536(4) . ? C24 H24 1 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C29 1.512(3) . ? C27 C28 1.513(4) . ? C27 H27 1 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 C35 1.405(3) . ? C30 C31 1.410(3) . ? C31 C32 1.391(3) . ? C31 C36 1.521(3) . ? C32 C33 1.382(3) . ? C32 H32 0.95 . ? C33 C34 1.381(3) . ? C33 H33 0.95 . ? C34 C35 1.391(3) . ? C34 H34 0.95 . ? C35 C39 1.522(3) . ? C36 C37 1.527(3) . ? C36 C38 1.532(3) . ? C36 H36 1 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 C41 1.513(4) . ? C39 C40 1.526(3) . ? C39 H39 1 . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 C43 1.478(4) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? C43 C44 1.489(4) . ? C43 H43A 0.99 . ? C43 H43B 0.99 . ? C44 C45 1.497(4) . ? C44 H44A 0.99 . ? C44 H44B 0.99 . ? C45 H45A 0.99 . ? C45 H45B 0.99 . ? C47 C48 1.512(3) . ? C47 C52 1.515(3) . ? C47 H47 1 . ? C48 C49 1.532(3) . ? C48 H48A 0.99 . ? C48 H48B 0.99 . ? C49 C50 1.514(4) . ? C49 H49A 0.99 . ? C49 H49B 0.99 . ? C50 C51 1.507(4) . ? C50 H50A 0.99 . ? C50 H50B 0.99 . ? C51 C52 1.529(3) . ? C51 H51A 0.99 . ? C51 H51B 0.99 . ? C52 H52A 0.99 . ? C52 H52B 0.99 . ? C53 C58 1.494(4) . ? C53 C54 1.552(4) . ? C53 H53 1 . ? C54 C55 1.545(5) . ? C54 H54A 0.99 . ? C54 H54B 0.99 . ? C55 C56 1.504(6) . ? C55 H55A 0.99 . ? C55 H55B 0.99 . ? C56 C57 1.496(6) . ? C56 H56A 0.99 . ? C56 H56B 0.99 . ? C57 C58 1.532(5) . ? C57 H57A 0.99 . ? C57 H57B 0.99 . ? C58 H58A 0.99 . ? C58 H58B 0.99 . ? C54A C55A 1.519(8) . ? C54A H54C 0.99 . ? C54A H54D 0.99 . ? C55A C56A 1.475(10) . ? C55A H55C 0.99 . ? C55A H55D 0.99 . ? C56A C57A 1.521(10) . ? C56A H56C 0.99 . ? C56A H56D 0.99 . ? C57A C58A 1.542(9) . ? C57A H57C 0.99 . ? C57A H57D 0.99 . ? C58A H58C 0.99 . ? C58A H58D 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ca N4 149.71(6) . . ? N2 Ca N1 80.65(5) . . ? N4 Ca N1 129.25(5) . . ? N2 Ca O 88.17(5) . . ? N4 Ca O 92.43(5) . . ? N1 Ca O 96.26(5) . . ? N2 Ca N5 112.00(5) . . ? N4 Ca N5 56.16(5) . . ? N1 Ca N5 113.45(5) . . ? O Ca N5 145.91(5) . . ? C42 O C45 109.09(18) . . ? C42 O Ca 120.09(14) . . ? C45 O Ca 130.79(14) . . ? C1 N1 C6 119.42(15) . . ? C1 N1 Ca 110.61(12) . . ? C6 N1 Ca 126.24(11) . . ? C3 N2 C18 120.31(15) . . ? C3 N2 Ca 111.69(11) . . ? C18 N2 Ca 125.14(11) . . ? C46 N3 C30 130.56(15) . . ? C46 N3 H3X 113.4(15) . . ? C30 N3 H3X 115.8(15) . . ? C46 N4 C47 121.98(14) . . ? C46 N4 Ca 94.11(10) . . ? C47 N4 Ca 143.20(11) . . ? C46 N5 C53 122.90(15) . . ? C46 N5 Ca 92.85(11) . . ? C53 N5 Ca 139.79(11) . . ? N1 C1 C2 125.34(17) . . ? N1 C1 C4 120.64(18) . . ? C2 C1 C4 114.01(18) . . ? C3 C2 C1 131.72(19) . . ? C3 C2 H2 114.1 . . ? C1 C2 H2 114.1 . . ? N2 C3 C2 124.10(17) . . ? N2 C3 C5 120.41(17) . . ? C2 C3 C5 115.48(18) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 119.60(18) . . ? C11 C6 N1 121.32(16) . . ? C7 C6 N1 118.95(17) . . ? C8 C7 C6 118.94(19) . . ? C8 C7 C12 119.9(2) . . ? C6 C7 C12 121.2(2) . . ? C9 C8 C7 121.4(2) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C10 C9 C8 119.5(2) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 121.7(2) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C10 C11 C6 118.83(18) . . ? C10 C11 C15 119.04(17) . . ? C6 C11 C15 122.13(17) . . ? C14 C12 C7 111.5(3) . . ? C14 C12 C13 111.1(3) . . ? C7 C12 C13 112.0(3) . . ? C14 C12 H12 107.3 . . ? C7 C12 H12 107.3 . . ? C13 C12 H12 107.3 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 111.35(19) . . ? C11 C15 C16 112.21(18) . . ? C17 C15 C16 109.64(18) . . ? C11 C15 H15 107.8 . . ? C17 C15 H15 107.8 . . ? C16 C15 H15 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 119.94(17) . . ? C23 C18 N2 119.72(16) . . ? C19 C18 N2 120.08(17) . . ? C20 C19 C18 118.65(19) . . ? C20 C19 C24 119.10(19) . . ? C18 C19 C24 122.24(18) . . ? C21 C20 C19 121.7(2) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C22 119.55(19) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C23 121.1(2) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 C18 119.07(18) . . ? C22 C23 C27 119.07(18) . . ? C18 C23 C27 121.87(17) . . ? C19 C24 C25 111.5(2) . . ? C19 C24 C26 110.9(2) . . ? C25 C24 C26 109.7(3) . . ? C19 C24 H24 108.2 . . ? C25 C24 H24 108.2 . . ? C26 C24 H24 108.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C23 111.85(19) . . ? C29 C27 C28 111.4(2) . . ? C23 C27 C28 111.67(19) . . ? C29 C27 H27 107.2 . . ? C23 C27 H27 107.2 . . ? C28 C27 H27 107.2 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 C31 121.09(16) . . ? C35 C30 N3 118.58(16) . . ? C31 C30 N3 120.29(16) . . ? C32 C31 C30 117.98(17) . . ? C32 C31 C36 120.91(17) . . ? C30 C31 C36 121.02(16) . . ? C33 C32 C31 121.36(18) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C34 C33 C32 119.88(18) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 121.16(18) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C34 C35 C30 118.30(17) . . ? C34 C35 C39 119.93(17) . . ? C30 C35 C39 121.73(17) . . ? C31 C36 C37 113.64(18) . . ? C31 C36 C38 110.09(16) . . ? C37 C36 C38 109.60(19) . . ? C31 C36 H36 107.8 . . ? C37 C36 H36 107.8 . . ? C38 C36 H36 107.8 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C41 C39 C35 109.96(19) . . ? C41 C39 C40 110.2(2) . . ? C35 C39 C40 112.7(2) . . ? C41 C39 H39 107.9 . . ? C35 C39 H39 107.9 . . ? C40 C39 H39 107.9 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O C42 C43 107.5(2) . . ? O C42 H42A 110.2 . . ? C43 C42 H42A 110.2 . . ? O C42 H42B 110.2 . . ? C43 C42 H42B 110.2 . . ? H42A C42 H42B 108.5 . . ? C42 C43 C44 105.3(2) . . ? C42 C43 H43A 110.7 . . ? C44 C43 H43A 110.7 . . ? C42 C43 H43B 110.7 . . ? C44 C43 H43B 110.7 . . ? H43A C43 H43B 108.8 . . ? C43 C44 C45 103.4(2) . . ? C43 C44 H44A 111.1 . . ? C45 C44 H44A 111.1 . . ? C43 C44 H44B 111.1 . . ? C45 C44 H44B 111.1 . . ? H44A C44 H44B 109 . . ? O C45 C44 105.9(2) . . ? O C45 H45A 110.6 . . ? C44 C45 H45A 110.6 . . ? O C45 H45B 110.6 . . ? C44 C45 H45B 110.6 . . ? H45A C45 H45B 108.7 . . ? N5 C46 N4 116.22(15) . . ? N5 C46 N3 124.75(16) . . ? N4 C46 N3 118.97(15) . . ? N5 C46 Ca 59.07(9) . . ? N4 C46 Ca 57.65(9) . . ? N3 C46 Ca 170.19(12) . . ? N4 C47 C48 111.34(16) . . ? N4 C47 C52 110.28(15) . . ? C48 C47 C52 110.87(18) . . ? N4 C47 H47 108.1 . . ? C48 C47 H47 108.1 . . ? C52 C47 H47 108.1 . . ? C47 C48 C49 113.31(19) . . ? C47 C48 H48A 108.9 . . ? C49 C48 H48A 108.9 . . ? C47 C48 H48B 108.9 . . ? C49 C48 H48B 108.9 . . ? H48A C48 H48B 107.7 . . ? C50 C49 C48 111.1(2) . . ? C50 C49 H49A 109.4 . . ? C48 C49 H49A 109.4 . . ? C50 C49 H49B 109.4 . . ? C48 C49 H49B 109.4 . . ? H49A C49 H49B 108 . . ? C51 C50 C49 110.31(19) . . ? C51 C50 H50A 109.6 . . ? C49 C50 H50A 109.6 . . ? C51 C50 H50B 109.6 . . ? C49 C50 H50B 109.6 . . ? H50A C50 H50B 108.1 . . ? C50 C51 C52 110.42(19) . . ? C50 C51 H51A 109.6 . . ? C52 C51 H51A 109.6 . . ? C50 C51 H51B 109.6 . . ? C52 C51 H51B 109.6 . . ? H51A C51 H51B 108.1 . . ? C47 C52 C51 112.25(17) . . ? C47 C52 H52A 109.2 . . ? C51 C52 H52A 109.2 . . ? C47 C52 H52B 109.2 . . ? C51 C52 H52B 109.2 . . ? H52A C52 H52B 107.9 . . ? N5 C53 C58 112.44(19) . . ? N5 C53 C54 108.70(18) . . ? C58 C53 C54 108.6(2) . . ? N5 C53 H53 109 . . ? C58 C53 H53 109 . . ? C54 C53 H53 109 . . ? C55 C54 C53 111.9(3) . . ? C55 C54 H54A 109.2 . . ? C53 C54 H54A 109.2 . . ? C55 C54 H54B 109.2 . . ? C53 C54 H54B 109.2 . . ? H54A C54 H54B 107.9 . . ? C56 C55 C54 111.0(4) . . ? C56 C55 H55A 109.4 . . ? C54 C55 H55A 109.4 . . ? C56 C55 H55B 109.4 . . ? C54 C55 H55B 109.4 . . ? H55A C55 H55B 108 . . ? C57 C56 C55 113.3(3) . . ? C57 C56 H56A 108.9 . . ? C55 C56 H56A 108.9 . . ? C57 C56 H56B 108.9 . . ? C55 C56 H56B 108.9 . . ? H56A C56 H56B 107.7 . . ? C56 C57 C58 110.1(4) . . ? C56 C57 H57A 109.6 . . ? C58 C57 H57A 109.6 . . ? C56 C57 H57B 109.6 . . ? C58 C57 H57B 109.6 . . ? H57A C57 H57B 108.2 . . ? C53 C58 C57 112.4(3) . . ? C53 C58 H58A 109.1 . . ? C57 C58 H58A 109.1 . . ? C53 C58 H58B 109.1 . . ? C57 C58 H58B 109.1 . . ? H58A C58 H58B 107.9 . . ? C55A C54A H54C 109 . . ? C55A C54A H54D 109 . . ? H54C C54A H54D 107.8 . . ? C56A C55A C54A 111.0(6) . . ? C56A C55A H55C 109.4 . . ? C54A C55A H55C 109.4 . . ? C56A C55A H55D 109.4 . . ? C54A C55A H55D 109.4 . . ? H55C C55A H55D 108 . . ? C55A C56A C57A 112.2(6) . . ? C55A C56A H56C 109.2 . . ? C57A C56A H56C 109.2 . . ? C55A C56A H56D 109.2 . . ? C57A C56A H56D 109.2 . . ? H56C C56A H56D 107.9 . . ? C56A C57A C58A 109.8(6) . . ? C56A C57A H57C 109.7 . . ? C58A C57A H57C 109.7 . . ? C56A C57A H57D 109.7 . . ? C58A C57A H57D 109.7 . . ? H57C C57A H57D 108.2 . . ? C57A C58A H58C 109.2 . . ? C57A C58A H58D 109.2 . . ? H58C C58A H58D 107.9 . . ? #===END data_(7)-oct1206 _database_code_depnum_ccdc_archive 'CCDC 667068' _audit_creation_date 2006-10-20T12:34:12-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C58 H81 Ca N5 O' _chemical_formula_sum 'C58 H81 Ca N5 O' _chemical_formula_weight 904.36 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.0903(3) _cell_length_b 19.8612(6) _cell_length_c 18.1455(6) _cell_angle_alpha 90 _cell_angle_beta 104.154(2) _cell_angle_gamma 90 _cell_volume 5273.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 24833 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9130 _exptl_absorpt_correction_T_max 0.9912 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.264263E-1 _diffrn_orient_matrix_ub_12 0.130677E-1 _diffrn_orient_matrix_ub_13 -0.433953E-1 _diffrn_orient_matrix_ub_21 -0.629709E-1 _diffrn_orient_matrix_ub_22 0.3446E-2 _diffrn_orient_matrix_ub_23 -0.33887E-1 _diffrn_orient_matrix_ub_31 -0.26459E-2 _diffrn_orient_matrix_ub_32 0.485018E-1 _diffrn_orient_matrix_ub_33 0.140995E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_unetI/netI 0.055 _diffrn_reflns_number 32780 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 10342 _reflns_number_gt 7206 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+2.7982P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10342 _refine_ls_number_parameters 596 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0867 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.498 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.044 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca Ca 0.06253(3) 0.19275(2) 0.71250(2) 0.02615(11) Uani 1 1 d . . . O O 0.17808(11) 0.26838(8) 0.77632(10) 0.0443(4) Uani 1 1 d . . . N1 N 0.16815(11) 0.10427(8) 0.70584(9) 0.0281(4) Uani 1 1 d . . . N2 N 0.08553(11) 0.21880(8) 0.59022(9) 0.0272(4) Uani 1 1 d . . . N3 N -0.19170(11) 0.18709(9) 0.77621(10) 0.0308(4) Uani 1 1 d . . . N4 N -0.08739(11) 0.15122(9) 0.70163(10) 0.0342(4) Uani 1 1 d . . . N5 N -0.04404(12) 0.23819(9) 0.78335(10) 0.0342(4) Uani 1 1 d . . . C1 C 0.12500(13) 0.06944(10) 0.64481(12) 0.0282(5) Uani 1 1 d . . . C2 C 0.06915(13) 0.09748(10) 0.57828(12) 0.0287(5) Uani 1 1 d . . . H2 H 0.0298 0.0659 0.5471 0.034 Uiso 1 1 calc R . . C3 C 0.06047(13) 0.16390(10) 0.54908(11) 0.0276(5) Uani 1 1 d . . . C4 C 0.13334(15) -0.00662(10) 0.64369(13) 0.0354(5) Uani 1 1 d . . . H4A H 0.1972 -0.0191 0.6478 0.053 Uiso 1 1 calc R . . H4B H 0.0951 -0.0242 0.596 0.053 Uiso 1 1 calc R . . H4C H 0.1131 -0.0258 0.6866 0.053 Uiso 1 1 calc R . . C5 C 0.01691(16) 0.16779(12) 0.46409(12) 0.0380(5) Uani 1 1 d . . . H5A H -0.0492 0.1608 0.455 0.057 Uiso 1 1 calc R . . H5B H 0.0431 0.1329 0.4377 0.057 Uiso 1 1 calc R . . H5C H 0.0287 0.2122 0.445 0.057 Uiso 1 1 calc R . . C6 C 0.23633(14) 0.06940(10) 0.76221(12) 0.0295(5) Uani 1 1 d . . . C7 C 0.32641(14) 0.06378(11) 0.75285(12) 0.0333(5) Uani 1 1 d . . . C8 C 0.39064(15) 0.02866(11) 0.80742(13) 0.0385(6) Uani 1 1 d . . . H8 H 0.4509 0.0236 0.801 0.046 Uiso 1 1 calc R . . C9 C 0.36921(15) 0.00096(11) 0.87057(13) 0.0392(6) Uani 1 1 d . . . H9 H 0.414 -0.0233 0.9067 0.047 Uiso 1 1 calc R . . C10 C 0.28250(15) 0.00885(11) 0.88070(13) 0.0370(5) Uani 1 1 d . . . H10 H 0.2684 -0.0091 0.925 0.044 Uiso 1 1 calc R . . C11 C 0.21469(14) 0.04252(10) 0.82749(12) 0.0321(5) Uani 1 1 d . . . C12 C 0.35574(15) 0.09376(12) 0.68544(14) 0.0422(6) Uani 1 1 d . . . H12 H 0.3027 0.1186 0.6531 0.051 Uiso 1 1 calc R . . C13 C 0.43528(18) 0.14362(14) 0.71188(18) 0.0619(8) Uani 1 1 d . . . H13A H 0.4172 0.1788 0.7432 0.093 Uiso 1 1 calc R . . H13B H 0.4505 0.1642 0.6674 0.093 Uiso 1 1 calc R . . H13C H 0.4888 0.1196 0.7418 0.093 Uiso 1 1 calc R . . C14 C 0.38533(19) 0.03918(15) 0.63707(15) 0.0570(7) Uani 1 1 d . . . H14A H 0.4385 0.0152 0.6676 0.086 Uiso 1 1 calc R . . H14B H 0.4015 0.06 0.5932 0.086 Uiso 1 1 calc R . . H14C H 0.335 0.0074 0.6194 0.086 Uiso 1 1 calc R . . C15 C 0.12002(15) 0.04938(11) 0.84206(13) 0.0356(5) Uani 1 1 d . . . H15 H 0.0789 0.0703 0.7961 0.043 Uiso 1 1 calc R . . C16 C 0.07922(17) -0.01828(12) 0.85566(15) 0.0473(6) Uani 1 1 d . . . H16A H 0.0798 -0.0486 0.8132 0.071 Uiso 1 1 calc R . . H16B H 0.0161 -0.0118 0.8595 0.071 Uiso 1 1 calc R . . H16C H 0.1155 -0.038 0.903 0.071 Uiso 1 1 calc R . . C17 C 0.12362(17) 0.09610(14) 0.90952(17) 0.0582(7) Uani 1 1 d . . . H17A H 0.0627 0.0991 0.9194 0.087 Uiso 1 1 calc R . . H17B H 0.1435 0.141 0.8979 0.087 Uiso 1 1 calc R . . H17C H 0.1669 0.0782 0.9545 0.087 Uiso 1 1 calc R . . C18 C 0.08775(14) 0.28037(10) 0.54904(11) 0.0283(5) Uani 1 1 d . . . C19 C 0.16816(14) 0.29689(10) 0.52665(12) 0.0305(5) Uani 1 1 d . . . C20 C 0.16699(16) 0.35336(11) 0.48059(13) 0.0364(5) Uani 1 1 d . . . H20 H 0.2202 0.3648 0.4642 0.044 Uiso 1 1 calc R . . C21 C 0.09002(16) 0.39281(12) 0.45856(13) 0.0410(6) Uani 1 1 d . . . H21 H 0.0895 0.4298 0.4252 0.049 Uiso 1 1 calc R . . C22 C 0.01385(16) 0.37871(11) 0.48488(13) 0.0391(5) Uani 1 1 d . . . H22 H -0.038 0.4074 0.4711 0.047 Uiso 1 1 calc R . . C23 C 0.01130(14) 0.32309(11) 0.53139(12) 0.0321(5) Uani 1 1 d . . . C24 C 0.25399(14) 0.25429(11) 0.55157(13) 0.0337(5) Uani 1 1 d . . . H24 H 0.2526 0.2335 0.6015 0.04 Uiso 1 1 calc R . . C25 C 0.34212(16) 0.29592(13) 0.56439(15) 0.0473(6) Uani 1 1 d . . . H25A H 0.3507 0.3114 0.5153 0.071 Uiso 1 1 calc R . . H25B H 0.3943 0.268 0.5897 0.071 Uiso 1 1 calc R . . H25C H 0.3377 0.3349 0.5964 0.071 Uiso 1 1 calc R . . C26 C 0.25814(16) 0.19680(12) 0.49678(15) 0.0468(6) Uani 1 1 d . . . H26A H 0.2053 0.1671 0.493 0.07 Uiso 1 1 calc R . . H26B H 0.3146 0.1711 0.5156 0.07 Uiso 1 1 calc R . . H26C H 0.2572 0.2153 0.4465 0.07 Uiso 1 1 calc R . . C27 C -0.07394(14) 0.31232(11) 0.56101(13) 0.0357(5) Uani 1 1 d . . . H27 H -0.0631 0.2724 0.5957 0.043 Uiso 1 1 calc R . . C28 C -0.15806(17) 0.29789(14) 0.49671(15) 0.0527(7) Uani 1 1 d . . . H28A H -0.1693 0.336 0.4614 0.079 Uiso 1 1 calc R . . H28B H -0.2113 0.2913 0.5179 0.079 Uiso 1 1 calc R . . H28C H -0.1476 0.2571 0.4696 0.079 Uiso 1 1 calc R . . C29 C -0.09121(17) 0.37335(13) 0.60671(15) 0.0479(6) Uani 1 1 d . . . H29A H -0.0368 0.3823 0.6477 0.072 Uiso 1 1 calc R . . H29B H -0.1434 0.3643 0.6285 0.072 Uiso 1 1 calc R . . H29C H -0.1045 0.4127 0.5732 0.072 Uiso 1 1 calc R . . C30 C -0.20605(14) 0.12747(11) 0.81471(12) 0.0322(5) Uani 1 1 d . . . C31 C -0.28634(15) 0.08973(11) 0.79258(13) 0.0375(5) Uani 1 1 d . . . H31 H -0.3354 0.1055 0.7529 0.045 Uiso 1 1 calc R . . C32 C -0.29426(17) 0.02949(12) 0.82856(15) 0.0461(6) Uani 1 1 d . . . H32 H -0.3486 0.0037 0.8128 0.055 Uiso 1 1 calc R . . C33 C -0.22442(19) 0.00634(13) 0.88695(16) 0.0511(7) Uani 1 1 d . . . H33 H -0.2305 -0.0352 0.9112 0.061 Uiso 1 1 calc R . . C34 C -0.14543(18) 0.04404(13) 0.91005(15) 0.0485(6) Uani 1 1 d . . . H34 H -0.0972 0.0285 0.9505 0.058 Uiso 1 1 calc R . . C35 C -0.13655(15) 0.10445(12) 0.87418(13) 0.0391(5) Uani 1 1 d . . . H35 H -0.0823 0.1303 0.8905 0.047 Uiso 1 1 calc R . . C36 C -0.26384(14) 0.23149(10) 0.74467(13) 0.0335(5) Uani 1 1 d . . . C37 C -0.26562(15) 0.26506(12) 0.67721(15) 0.0432(6) Uani 1 1 d . . . H37 H -0.2192 0.2568 0.6512 0.052 Uiso 1 1 calc R . . C38 C -0.33477(18) 0.31052(13) 0.64757(17) 0.0570(7) Uani 1 1 d . . . H38 H -0.3354 0.3332 0.6014 0.068 Uiso 1 1 calc R . . C39 C -0.40290(18) 0.32310(14) 0.6847(2) 0.0652(9) Uani 1 1 d . . . H39 H -0.4502 0.3544 0.6643 0.078 Uiso 1 1 calc R . . C40 C -0.40146(17) 0.28978(14) 0.75175(19) 0.0594(8) Uani 1 1 d . . . H40 H -0.4483 0.298 0.7773 0.071 Uiso 1 1 calc R . . C41 C -0.33261(15) 0.24466(12) 0.78197(15) 0.0439(6) Uani 1 1 d . . . H41 H -0.332 0.2224 0.8284 0.053 Uiso 1 1 calc R . . C42 C 0.16610(18) 0.33944(13) 0.76146(19) 0.0607(8) Uani 1 1 d . . . H42A H 0.1661 0.3643 0.8088 0.073 Uiso 1 1 calc R . . H42B H 0.1077 0.3483 0.7238 0.073 Uiso 1 1 calc R . . C43 C 0.24454(17) 0.36009(13) 0.73118(15) 0.0489(6) Uani 1 1 d . . . H43A H 0.2584 0.4085 0.7403 0.059 Uiso 1 1 calc R . . H43B H 0.2329 0.3508 0.676 0.059 Uiso 1 1 calc R . . C44 C 0.32021(17) 0.31707(13) 0.77566(19) 0.0618(8) Uani 1 1 d . . . H44A H 0.3472 0.3369 0.8262 0.074 Uiso 1 1 calc R . . H44B H 0.3688 0.311 0.7482 0.074 Uiso 1 1 calc R . . C45 C 0.27349(17) 0.25162(14) 0.78280(18) 0.0602(8) Uani 1 1 d . . . H45A H 0.2793 0.2202 0.7419 0.072 Uiso 1 1 calc R . . H45B H 0.3006 0.2303 0.8325 0.072 Uiso 1 1 calc R . . C46 C -0.10560(13) 0.19256(11) 0.75313(12) 0.0293(5) Uani 1 1 d . . . C47 C -0.05530(14) 0.28138(10) 0.84582(12) 0.0320(5) Uani 1 1 d . . . H47 H -0.1091 0.2651 0.8637 0.038 Uiso 1 1 calc R . . C48 C -0.07228(15) 0.35449(11) 0.81991(13) 0.0366(5) Uani 1 1 d . . . H48A H -0.0222 0.3696 0.7973 0.044 Uiso 1 1 calc R . . H48B H -0.1302 0.3572 0.78 0.044 Uiso 1 1 calc R . . C49 C -0.07784(15) 0.40161(11) 0.88504(14) 0.0404(6) Uani 1 1 d . . . H49A H -0.132 0.3899 0.9041 0.049 Uiso 1 1 calc R . . H49B H -0.0852 0.4486 0.8662 0.049 Uiso 1 1 calc R . . C50 C 0.00806(16) 0.39637(12) 0.94984(14) 0.0423(6) Uani 1 1 d . . . H50A H 0.0613 0.4128 0.9322 0.051 Uiso 1 1 calc R . . H50B H 0.0012 0.4253 0.9925 0.051 Uiso 1 1 calc R . . C51 C 0.02503(16) 0.32419(11) 0.97733(13) 0.0401(6) Uani 1 1 d . . . H51A H -0.0248 0.3095 1.0004 0.048 Uiso 1 1 calc R . . H51B H 0.0832 0.3218 1.0169 0.048 Uiso 1 1 calc R . . C52 C 0.02971(15) 0.27698(11) 0.91185(13) 0.0366(5) Uani 1 1 d . . . H52A H 0.0369 0.2301 0.9309 0.044 Uiso 1 1 calc R . . H52B H 0.0842 0.2884 0.8931 0.044 Uiso 1 1 calc R . . C53 C -0.15467(14) 0.10249(11) 0.66094(12) 0.0331(5) Uani 1 1 d . . . H53 H -0.2129 0.1091 0.6771 0.04 Uiso 1 1 calc R . . C54 C -0.12096(15) 0.03088(11) 0.68131(14) 0.0399(6) Uani 1 1 d . . . H54A H -0.0609 0.0248 0.6693 0.048 Uiso 1 1 calc R . . H54B H -0.1125 0.0239 0.7366 0.048 Uiso 1 1 calc R . . C55 C -0.18769(17) -0.02130(13) 0.63825(15) 0.0492(6) Uani 1 1 d . . . H55A H -0.1615 -0.0669 0.6502 0.059 Uiso 1 1 calc R . . H55B H -0.2453 -0.019 0.655 0.059 Uiso 1 1 calc R . . C56 C -0.20808(18) -0.00980(13) 0.55306(15) 0.0517(7) Uani 1 1 d . . . H56A H -0.2551 -0.0423 0.5269 0.062 Uiso 1 1 calc R . . H56B H -0.152 -0.0178 0.5352 0.062 Uiso 1 1 calc R . . C57 C -0.24189(16) 0.06159(12) 0.53269(14) 0.0451(6) Uani 1 1 d . . . H57A H -0.3016 0.0679 0.5453 0.054 Uiso 1 1 calc R . . H57B H -0.2509 0.0686 0.4773 0.054 Uiso 1 1 calc R . . C58 C -0.17410(15) 0.11342(11) 0.57557(13) 0.0371(5) Uani 1 1 d . . . H58A H -0.1163 0.1101 0.5592 0.044 Uiso 1 1 calc R . . H58B H -0.1992 0.1592 0.5631 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca 0.0261(2) 0.0253(2) 0.0287(2) -0.00037(18) 0.00980(16) -0.00013(18) O 0.0461(9) 0.0368(9) 0.0561(11) -0.0107(8) 0.0240(8) -0.0121(8) N1 0.0278(9) 0.0246(9) 0.0308(10) 0.0003(8) 0.0054(7) 0.0004(7) N2 0.0286(9) 0.0252(9) 0.0289(9) 0.0020(8) 0.0093(7) 0.0010(7) N3 0.0265(9) 0.0308(10) 0.0381(10) -0.0010(8) 0.0135(8) -0.0013(8) N4 0.0305(9) 0.0370(11) 0.0370(11) -0.0112(9) 0.0115(8) -0.0057(8) N5 0.0330(10) 0.0330(10) 0.0398(11) -0.0086(8) 0.0147(8) -0.0044(8) C1 0.0251(10) 0.0250(11) 0.0358(12) -0.0007(9) 0.0103(9) -0.0009(9) C2 0.0281(10) 0.0264(11) 0.0309(11) -0.0026(9) 0.0058(9) -0.0025(9) C3 0.0242(10) 0.0305(11) 0.0287(11) -0.0002(9) 0.0075(8) 0.0005(9) C4 0.0386(12) 0.0254(11) 0.0382(13) -0.0010(10) 0.0016(10) 0.0012(10) C5 0.0442(13) 0.0353(12) 0.0311(12) 0.0004(10) 0.0028(10) -0.0006(11) C6 0.0319(11) 0.0211(10) 0.0324(12) -0.0036(9) 0.0017(9) 0.0009(9) C7 0.0319(11) 0.0281(11) 0.0374(13) -0.0048(10) 0.0037(10) 0.0007(9) C8 0.0305(11) 0.0370(13) 0.0451(14) -0.0094(11) 0.0032(10) 0.0036(10) C9 0.0387(13) 0.0352(13) 0.0362(13) -0.0028(10) -0.0051(10) 0.0088(10) C10 0.0427(13) 0.0318(12) 0.0336(13) 0.0025(10) 0.0037(10) 0.0040(10) C11 0.0331(11) 0.0251(11) 0.0354(13) -0.0021(9) 0.0034(10) -0.0008(9) C12 0.0321(12) 0.0470(14) 0.0479(15) 0.0056(12) 0.0102(10) 0.0039(11) C13 0.0551(17) 0.0521(17) 0.085(2) -0.0005(16) 0.0290(15) -0.0101(14) C14 0.0577(16) 0.0706(19) 0.0465(16) -0.0086(14) 0.0198(13) -0.0015(14) C15 0.0362(12) 0.0329(12) 0.0367(13) 0.0063(10) 0.0072(10) 0.0024(10) C16 0.0498(14) 0.0426(14) 0.0529(16) 0.0051(12) 0.0192(12) -0.0025(12) C17 0.0431(14) 0.0556(17) 0.077(2) -0.0166(15) 0.0173(14) 0.0068(13) C18 0.0362(11) 0.0267(11) 0.0222(10) 0.0001(9) 0.0079(9) 0.0004(9) C19 0.0381(12) 0.0281(11) 0.0275(11) -0.0031(9) 0.0119(9) -0.0007(9) C20 0.0444(13) 0.0338(12) 0.0359(13) 0.0034(10) 0.0193(10) -0.0030(11) C21 0.0579(15) 0.0325(13) 0.0373(13) 0.0095(10) 0.0211(11) 0.0043(12) C22 0.0464(13) 0.0337(13) 0.0394(13) 0.0074(10) 0.0149(11) 0.0092(11) C23 0.0373(12) 0.0311(12) 0.0293(11) 0.0027(9) 0.0110(9) 0.0030(10) C24 0.0340(11) 0.0342(12) 0.0358(12) 0.0011(10) 0.0142(10) -0.0007(10) C25 0.0397(13) 0.0465(15) 0.0576(16) 0.0004(12) 0.0154(12) -0.0030(11) C26 0.0429(13) 0.0426(14) 0.0575(16) -0.0073(13) 0.0172(12) 0.0044(12) C27 0.0351(12) 0.0355(13) 0.0377(13) 0.0115(10) 0.0116(10) 0.0093(10) C28 0.0427(14) 0.0605(17) 0.0526(16) 0.0066(14) 0.0072(12) 0.0009(13) C29 0.0472(14) 0.0518(16) 0.0513(16) 0.0023(12) 0.0244(12) 0.0077(12) C30 0.0335(11) 0.0331(12) 0.0359(12) -0.0046(10) 0.0197(10) -0.0011(10) C31 0.0370(12) 0.0378(13) 0.0418(14) -0.0058(11) 0.0174(10) -0.0039(10) C32 0.0502(15) 0.0380(14) 0.0585(17) -0.0064(12) 0.0293(13) -0.0100(12) C33 0.0643(17) 0.0383(14) 0.0623(18) 0.0087(13) 0.0377(15) 0.0021(13) C34 0.0525(15) 0.0526(16) 0.0459(15) 0.0120(12) 0.0228(12) 0.0138(13) C35 0.0367(12) 0.0439(14) 0.0409(13) 0.0010(11) 0.0172(10) 0.0018(11) C36 0.0281(11) 0.0273(11) 0.0450(14) -0.0056(10) 0.0088(10) -0.0026(9) C37 0.0343(12) 0.0388(13) 0.0568(16) 0.0047(12) 0.0113(11) 0.0033(11) C38 0.0482(15) 0.0448(16) 0.073(2) 0.0155(14) 0.0060(14) 0.0040(13) C39 0.0384(15) 0.0452(16) 0.107(3) 0.0060(17) 0.0093(16) 0.0122(13) C40 0.0387(14) 0.0493(16) 0.094(2) -0.0100(16) 0.0248(15) 0.0059(13) C41 0.0353(12) 0.0408(14) 0.0593(16) -0.0078(12) 0.0188(12) 0.0020(11) C42 0.0507(16) 0.0388(15) 0.094(2) -0.0113(15) 0.0204(15) -0.0009(13) C43 0.0595(16) 0.0398(14) 0.0454(15) -0.0009(12) 0.0088(13) -0.0116(13) C44 0.0384(14) 0.0464(16) 0.092(2) 0.0031(15) -0.0011(14) -0.0125(12) C45 0.0467(15) 0.0515(17) 0.072(2) 0.0104(15) -0.0051(14) -0.0044(13) C46 0.0262(10) 0.0317(11) 0.0316(11) 0.0028(10) 0.0099(9) 0.0026(9) C47 0.0322(11) 0.0304(11) 0.0372(12) -0.0075(10) 0.0155(10) -0.0039(10) C48 0.0334(11) 0.0366(13) 0.0399(13) -0.0040(10) 0.0091(10) 0.0012(10) C49 0.0404(13) 0.0320(12) 0.0520(15) -0.0047(11) 0.0173(11) 0.0034(10) C50 0.0464(14) 0.0366(13) 0.0458(14) -0.0132(11) 0.0145(11) -0.0051(11) C51 0.0430(13) 0.0399(13) 0.0383(13) -0.0051(11) 0.0118(11) -0.0013(11) C52 0.0385(12) 0.0320(12) 0.0412(13) -0.0017(10) 0.0133(10) 0.0010(10) C53 0.0271(11) 0.0376(13) 0.0366(12) -0.0085(10) 0.0119(9) -0.0048(10) C54 0.0374(12) 0.0409(14) 0.0406(14) 0.0004(11) 0.0080(10) -0.0037(11) C55 0.0527(15) 0.0377(14) 0.0549(17) -0.0039(12) 0.0088(13) -0.0098(12) C56 0.0539(15) 0.0447(15) 0.0527(17) -0.0167(13) 0.0057(13) -0.0065(13) C57 0.0418(13) 0.0513(15) 0.0379(14) -0.0099(12) 0.0015(11) -0.0007(12) C58 0.0361(12) 0.0354(12) 0.0387(13) -0.0044(10) 0.0074(10) -0.0004(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca N4 2.3705(17) . ? Ca O 2.3771(16) . ? Ca N2 2.3849(17) . ? Ca N1 2.3953(17) . ? Ca N5 2.4626(17) . ? O C42 1.440(3) . ? O C45 1.454(3) . ? N1 C1 1.333(3) . ? N1 C6 1.439(3) . ? N2 C3 1.323(3) . ? N2 C18 1.438(3) . ? N3 C36 1.409(3) . ? N3 C30 1.418(3) . ? N3 C46 1.463(2) . ? N4 C46 1.322(3) . ? N4 C53 1.465(3) . ? N5 C46 1.318(3) . ? N5 C47 1.464(3) . ? C1 C2 1.407(3) . ? C1 C4 1.517(3) . ? C2 C3 1.416(3) . ? C2 H2 0.95 . ? C3 C5 1.523(3) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C11 1.409(3) . ? C6 C7 1.415(3) . ? C7 C8 1.392(3) . ? C7 C12 1.520(3) . ? C8 C9 1.379(3) . ? C8 H8 0.95 . ? C9 C10 1.374(3) . ? C9 H9 0.95 . ? C10 C11 1.394(3) . ? C10 H10 0.95 . ? C11 C15 1.521(3) . ? C12 C14 1.528(3) . ? C12 C13 1.540(3) . ? C12 H12 1 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C16 1.523(3) . ? C15 C17 1.526(3) . ? C15 H15 1 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C23 1.404(3) . ? C18 C19 1.409(3) . ? C19 C20 1.396(3) . ? C19 C24 1.520(3) . ? C20 C21 1.377(3) . ? C20 H20 0.95 . ? C21 C22 1.377(3) . ? C21 H21 0.95 . ? C22 C23 1.396(3) . ? C22 H22 0.95 . ? C23 C27 1.526(3) . ? C24 C26 1.525(3) . ? C24 C25 1.535(3) . ? C24 H24 1 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C29 1.527(3) . ? C27 C28 1.527(3) . ? C27 H27 1 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 C35 1.386(3) . ? C30 C31 1.398(3) . ? C31 C32 1.382(3) . ? C31 H31 0.95 . ? C32 C33 1.378(4) . ? C32 H32 0.95 . ? C33 C34 1.383(4) . ? C33 H33 0.95 . ? C34 C35 1.387(3) . ? C34 H34 0.95 . ? C35 H35 0.95 . ? C36 C37 1.388(3) . ? C36 C41 1.395(3) . ? C37 C38 1.385(3) . ? C37 H37 0.95 . ? C38 C39 1.383(4) . ? C38 H38 0.95 . ? C39 C40 1.380(4) . ? C39 H39 0.95 . ? C40 C41 1.380(4) . ? C40 H40 0.95 . ? C41 H41 0.95 . ? C42 C43 1.480(4) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? C43 C44 1.495(4) . ? C43 H43A 0.99 . ? C43 H43B 0.99 . ? C44 C45 1.499(4) . ? C44 H44A 0.99 . ? C44 H44B 0.99 . ? C45 H45A 0.99 . ? C45 H45B 0.99 . ? C47 C48 1.528(3) . ? C47 C52 1.529(3) . ? C47 H47 1 . ? C48 C49 1.526(3) . ? C48 H48A 0.99 . ? C48 H48B 0.99 . ? C49 C50 1.526(3) . ? C49 H49A 0.99 . ? C49 H49B 0.99 . ? C50 C51 1.519(3) . ? C50 H50A 0.99 . ? C50 H50B 0.99 . ? C51 C52 1.529(3) . ? C51 H51A 0.99 . ? C51 H51B 0.99 . ? C52 H52A 0.99 . ? C52 H52B 0.99 . ? C53 C58 1.520(3) . ? C53 C54 1.525(3) . ? C53 H53 1 . ? C54 C55 1.521(3) . ? C54 H54A 0.99 . ? C54 H54B 0.99 . ? C55 C56 1.518(4) . ? C55 H55A 0.99 . ? C55 H55B 0.99 . ? C56 C57 1.522(3) . ? C56 H56A 0.99 . ? C56 H56B 0.99 . ? C57 C58 1.524(3) . ? C57 H57A 0.99 . ? C57 H57B 0.99 . ? C58 H58A 0.99 . ? C58 H58B 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ca O 146.29(6) . . ? N4 Ca N2 110.56(6) . . ? O Ca N2 93.43(6) . . ? N4 Ca N1 111.95(6) . . ? O Ca N1 94.03(6) . . ? N2 Ca N1 82.08(6) . . ? N4 Ca N5 55.89(6) . . ? O Ca N5 90.51(6) . . ? N2 Ca N5 131.94(6) . . ? N1 Ca N5 145.36(6) . . ? C42 O C45 108.42(18) . . ? C42 O Ca 118.98(15) . . ? C45 O Ca 119.24(14) . . ? C1 N1 C6 117.40(16) . . ? C1 N1 Ca 103.11(12) . . ? C6 N1 Ca 133.34(13) . . ? C3 N2 C18 116.57(16) . . ? C3 N2 Ca 105.05(12) . . ? C18 N2 Ca 134.05(13) . . ? C36 N3 C30 121.79(17) . . ? C36 N3 C46 119.29(17) . . ? C30 N3 C46 117.13(16) . . ? C46 N4 C53 121.88(17) . . ? C46 N4 Ca 94.83(12) . . ? C53 N4 Ca 143.28(13) . . ? C46 N5 C47 121.44(17) . . ? C46 N5 Ca 90.84(12) . . ? C47 N5 Ca 146.42(13) . . ? N1 C1 C2 125.17(19) . . ? N1 C1 C4 120.18(18) . . ? C2 C1 C4 114.64(18) . . ? C1 C2 C3 132.14(19) . . ? C1 C2 H2 113.9 . . ? C3 C2 H2 113.9 . . ? N2 C3 C2 124.69(18) . . ? N2 C3 C5 121.49(18) . . ? C2 C3 C5 113.81(18) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 119.87(19) . . ? C11 C6 N1 120.52(18) . . ? C7 C6 N1 119.59(19) . . ? C8 C7 C6 118.5(2) . . ? C8 C7 C12 118.66(19) . . ? C6 C7 C12 122.88(19) . . ? C9 C8 C7 121.8(2) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C10 C9 C8 119.4(2) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 121.6(2) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C6 118.8(2) . . ? C10 C11 C15 119.0(2) . . ? C6 C11 C15 122.20(18) . . ? C7 C12 C14 111.6(2) . . ? C7 C12 C13 111.1(2) . . ? C14 C12 C13 108.7(2) . . ? C7 C12 H12 108.5 . . ? C14 C12 H12 108.5 . . ? C13 C12 H12 108.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 112.53(18) . . ? C11 C15 C17 110.06(19) . . ? C16 C15 C17 110.0(2) . . ? C11 C15 H15 108 . . ? C16 C15 H15 108 . . ? C17 C15 H15 108 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 120.71(19) . . ? C23 C18 N2 120.67(18) . . ? C19 C18 N2 118.62(18) . . ? C20 C19 C18 118.28(19) . . ? C20 C19 C24 120.69(19) . . ? C18 C19 C24 121.03(18) . . ? C21 C20 C19 121.1(2) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 120.0(2) . . ? C20 C21 H21 120 . . ? C22 C21 H21 120 . . ? C21 C22 C23 121.3(2) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 118.25(19) . . ? C22 C23 C27 118.29(19) . . ? C18 C23 C27 123.46(18) . . ? C19 C24 C26 112.98(18) . . ? C19 C24 C25 112.88(18) . . ? C26 C24 C25 109.27(18) . . ? C19 C24 H24 107.1 . . ? C26 C24 H24 107.1 . . ? C25 C24 H24 107.1 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 110.53(19) . . ? C23 C27 C28 111.85(19) . . ? C29 C27 C28 110.11(19) . . ? C23 C27 H27 108.1 . . ? C29 C27 H27 108.1 . . ? C28 C27 H27 108.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 C31 119.0(2) . . ? C35 C30 N3 118.78(19) . . ? C31 C30 N3 122.2(2) . . ? C32 C31 C30 119.8(2) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C33 C32 C31 120.9(2) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C34 119.5(2) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C33 C34 C35 120.1(2) . . ? C33 C34 H34 120 . . ? C35 C34 H34 120 . . ? C30 C35 C34 120.6(2) . . ? C30 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C37 C36 C41 118.8(2) . . ? C37 C36 N3 120.34(19) . . ? C41 C36 N3 120.8(2) . . ? C38 C37 C36 120.4(2) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C39 C38 C37 120.5(3) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C40 C39 C38 119.3(2) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C39 C40 C41 120.6(3) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C40 C41 C36 120.4(3) . . ? C40 C41 H41 119.8 . . ? C36 C41 H41 119.8 . . ? O C42 C43 105.4(2) . . ? O C42 H42A 110.7 . . ? C43 C42 H42A 110.7 . . ? O C42 H42B 110.7 . . ? C43 C42 H42B 110.7 . . ? H42A C42 H42B 108.8 . . ? C42 C43 C44 102.5(2) . . ? C42 C43 H43A 111.3 . . ? C44 C43 H43A 111.3 . . ? C42 C43 H43B 111.3 . . ? C44 C43 H43B 111.3 . . ? H43A C43 H43B 109.2 . . ? C43 C44 C45 103.2(2) . . ? C43 C44 H44A 111.1 . . ? C45 C44 H44A 111.1 . . ? C43 C44 H44B 111.1 . . ? C45 C44 H44B 111.1 . . ? H44A C44 H44B 109.1 . . ? O C45 C44 105.8(2) . . ? O C45 H45A 110.6 . . ? C44 C45 H45A 110.6 . . ? O C45 H45B 110.6 . . ? C44 C45 H45B 110.6 . . ? H45A C45 H45B 108.7 . . ? N5 C46 N4 118.29(18) . . ? N5 C46 N3 121.13(18) . . ? N4 C46 N3 120.58(18) . . ? N5 C46 Ca 61.20(10) . . ? N4 C46 Ca 57.21(10) . . ? N3 C46 Ca 175.59(14) . . ? N5 C47 C48 111.15(18) . . ? N5 C47 C52 109.83(17) . . ? C48 C47 C52 109.93(17) . . ? N5 C47 H47 108.6 . . ? C48 C47 H47 108.6 . . ? C52 C47 H47 108.6 . . ? C49 C48 C47 112.41(19) . . ? C49 C48 H48A 109.1 . . ? C47 C48 H48A 109.1 . . ? C49 C48 H48B 109.1 . . ? C47 C48 H48B 109.1 . . ? H48A C48 H48B 107.9 . . ? C48 C49 C50 110.97(18) . . ? C48 C49 H49A 109.4 . . ? C50 C49 H49A 109.4 . . ? C48 C49 H49B 109.4 . . ? C50 C49 H49B 109.4 . . ? H49A C49 H49B 108 . . ? C51 C50 C49 111.14(19) . . ? C51 C50 H50A 109.4 . . ? C49 C50 H50A 109.4 . . ? C51 C50 H50B 109.4 . . ? C49 C50 H50B 109.4 . . ? H50A C50 H50B 108 . . ? C50 C51 C52 111.09(19) . . ? C50 C51 H51A 109.4 . . ? C52 C51 H51A 109.4 . . ? C50 C51 H51B 109.4 . . ? C52 C51 H51B 109.4 . . ? H51A C51 H51B 108 . . ? C51 C52 C47 112.62(18) . . ? C51 C52 H52A 109.1 . . ? C47 C52 H52A 109.1 . . ? C51 C52 H52B 109.1 . . ? C47 C52 H52B 109.1 . . ? H52A C52 H52B 107.8 . . ? N4 C53 C58 110.88(17) . . ? N4 C53 C54 110.18(17) . . ? C58 C53 C54 110.49(18) . . ? N4 C53 H53 108.4 . . ? C58 C53 H53 108.4 . . ? C54 C53 H53 108.4 . . ? C55 C54 C53 111.78(19) . . ? C55 C54 H54A 109.3 . . ? C53 C54 H54A 109.3 . . ? C55 C54 H54B 109.3 . . ? C53 C54 H54B 109.3 . . ? H54A C54 H54B 107.9 . . ? C56 C55 C54 111.4(2) . . ? C56 C55 H55A 109.4 . . ? C54 C55 H55A 109.4 . . ? C56 C55 H55B 109.4 . . ? C54 C55 H55B 109.4 . . ? H55A C55 H55B 108 . . ? C55 C56 C57 111.1(2) . . ? C55 C56 H56A 109.4 . . ? C57 C56 H56A 109.4 . . ? C55 C56 H56B 109.4 . . ? C57 C56 H56B 109.4 . . ? H56A C56 H56B 108 . . ? C56 C57 C58 111.22(19) . . ? C56 C57 H57A 109.4 . . ? C58 C57 H57A 109.4 . . ? C56 C57 H57B 109.4 . . ? C58 C57 H57B 109.4 . . ? H57A C57 H57B 108 . . ? C53 C58 C57 111.22(19) . . ? C53 C58 H58A 109.4 . . ? C57 C58 H58A 109.4 . . ? C53 C58 H58B 109.4 . . ? C57 C58 H58B 109.4 . . ? H58A C58 H58B 108 . . ? #===END data_(8)-dec706 _database_code_depnum_ccdc_archive 'CCDC 667069' _audit_creation_date 2006-12-08T15:06:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C43 H71 Ca N5 O2' _chemical_formula_sum 'C43 H71 Ca N5 O2' _chemical_formula_weight 730.13 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6498(3) _cell_length_b 11.6365(3) _cell_length_c 19.3576(3) _cell_angle_alpha 98.220(1) _cell_angle_beta 90.253(1) _cell_angle_gamma 115.174(1) _cell_volume 2143.06(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20087 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.186 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8902 _exptl_absorpt_correction_T_max 0.9709 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.364269E-1 _diffrn_orient_matrix_ub_12 -0.327963E-1 _diffrn_orient_matrix_ub_13 -0.420967E-1 _diffrn_orient_matrix_ub_21 -0.854449E-1 _diffrn_orient_matrix_ub_22 -0.834691E-1 _diffrn_orient_matrix_ub_23 -0.58445E-2 _diffrn_orient_matrix_ub_31 -0.468433E-1 _diffrn_orient_matrix_ub_32 0.347976E-1 _diffrn_orient_matrix_ub_33 -0.305386E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_unetI/netI 0.036 _diffrn_reflns_number 31745 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 26 _diffrn_reflns_theta_full 26 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 8373 _reflns_number_gt 7247 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H on N4 was refined; other Hatomswere in riding mode. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+2.8388P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 8373 _refine_ls_number_parameters 479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1639 _refine_ls_wR_factor_gt 0.1592 _refine_ls_goodness_of_fit_ref 1.214 _refine_ls_restrained_S_all 1.214 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.467 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.067 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca Ca 0.34677(5) 0.29818(5) 0.24645(3) 0.01954(14) Uani 1 1 d . . . O1 O 0.57388(19) 0.46858(19) 0.31523(10) 0.0290(4) Uani 1 1 d . . . O3 O 0.3676(2) 0.2098(2) 0.35202(10) 0.0356(5) Uani 1 1 d . . . N1 N 0.2579(2) 0.45873(19) 0.25268(11) 0.0191(4) Uani 1 1 d . . . N2 N 0.0993(2) 0.16775(19) 0.25246(11) 0.0207(4) Uani 1 1 d . . . N3 N 0.3801(2) 0.2603(2) 0.12381(11) 0.0264(5) Uani 1 1 d . . . N4 N 0.6170(3) 0.3474(2) 0.09199(13) 0.0309(5) Uani 1 1 d . . . H4X H 0.587(4) 0.359(3) 0.053(2) 0.047(10) Uiso 1 1 d . . . N5 N 0.5509(2) 0.2865(2) 0.20357(11) 0.0248(5) Uani 1 1 d . . . C1 C 0.1467(3) 0.4293(2) 0.21060(13) 0.0205(5) Uani 1 1 d . . . C2 C 0.0483(3) 0.3027(2) 0.18390(13) 0.0232(5) Uani 1 1 d . . . H2 H -0.0077 0.2963 0.1439 0.028 Uiso 1 1 calc R . . C3 C 0.0188(3) 0.1845(2) 0.20620(13) 0.0225(5) Uani 1 1 d . . . C4 C 0.1154(3) 0.5338(3) 0.18681(15) 0.0296(6) Uani 1 1 d . . . H4C H 0.131 0.5355 0.137 0.044 Uiso 1 1 calc R . . H4B H 0.1767 0.6174 0.2141 0.044 Uiso 1 1 calc R . . H4A H 0.0182 0.516 0.194 0.044 Uiso 1 1 calc R . . C5 C -0.1142(3) 0.0726(3) 0.17253(16) 0.0325(6) Uani 1 1 d . . . H5C H -0.1473 0.0068 0.203 0.049 Uiso 1 1 calc R . . H5B H -0.0958 0.0356 0.1272 0.049 Uiso 1 1 calc R . . H5A H -0.1853 0.1033 0.1657 0.049 Uiso 1 1 calc R . . C6 C 0.3342(3) 0.5891(2) 0.28641(13) 0.0201(5) Uani 1 1 d . . . C7 C 0.2999(3) 0.6243(2) 0.35408(14) 0.0237(5) Uani 1 1 d . . . C8 C 0.3737(3) 0.7499(3) 0.38854(15) 0.0301(6) Uani 1 1 d . . . H8 H 0.3482 0.7753 0.4331 0.036 Uiso 1 1 calc R . . C9 C 0.4835(3) 0.8382(3) 0.35881(16) 0.0361(7) Uani 1 1 d . . . H9 H 0.5334 0.9235 0.383 0.043 Uiso 1 1 calc R . . C10 C 0.5207(3) 0.8021(3) 0.29375(16) 0.0336(7) Uani 1 1 d . . . H10 H 0.5976 0.8629 0.2741 0.04 Uiso 1 1 calc R . . C11 C 0.4477(3) 0.6784(3) 0.25648(14) 0.0267(6) Uani 1 1 d . . . C12 C 0.1851(3) 0.5259(3) 0.38928(14) 0.0273(6) Uani 1 1 d . . . H12 H 0.1748 0.4389 0.3673 0.033 Uiso 1 1 calc R . . C13 C 0.0466(3) 0.5299(4) 0.37688(18) 0.0446(8) Uani 1 1 d . . . H13C H 0.0546 0.6159 0.3953 0.067 Uiso 1 1 calc R . . H13B H -0.0245 0.4662 0.4008 0.067 Uiso 1 1 calc R . . H13A H 0.02 0.5102 0.3266 0.067 Uiso 1 1 calc R . . C14 C 0.2202(4) 0.5403(3) 0.46743(16) 0.0405(7) Uani 1 1 d . . . H14C H 0.1515 0.4663 0.486 0.061 Uiso 1 1 calc R . . H14B H 0.2185 0.6195 0.4916 0.061 Uiso 1 1 calc R . . H14A H 0.3131 0.5441 0.4749 0.061 Uiso 1 1 calc R . . C15 C 0.4945(3) 0.6447(3) 0.18526(15) 0.0339(7) Uani 1 1 d . . . H15 H 0.4357 0.5514 0.1677 0.041 Uiso 1 1 calc R . . C16 C 0.6457(4) 0.6663(3) 0.18985(18) 0.0446(8) Uani 1 1 d . . . H16C H 0.7058 0.7583 0.2035 0.067 Uiso 1 1 calc R . . H16B H 0.6693 0.6357 0.1442 0.067 Uiso 1 1 calc R . . H16A H 0.6594 0.6187 0.2248 0.067 Uiso 1 1 calc R . . C17 C 0.4748(4) 0.7224(4) 0.13206(18) 0.0511(9) Uani 1 1 d . . . H17C H 0.5034 0.6969 0.0866 0.077 Uiso 1 1 calc R . . H17B H 0.5318 0.8144 0.1482 0.077 Uiso 1 1 calc R . . H17A H 0.3767 0.7058 0.1274 0.077 Uiso 1 1 calc R . . C18 C 0.0474(3) 0.0513(2) 0.28183(14) 0.0244(5) Uani 1 1 d . . . C19 C -0.0180(3) 0.0480(3) 0.34516(15) 0.0279(6) Uani 1 1 d . . . C20 C -0.0553(3) -0.0604(3) 0.37762(16) 0.0360(7) Uani 1 1 d . . . H20 H -0.0999 -0.0638 0.4202 0.043 Uiso 1 1 calc R . . C21 C -0.0288(4) -0.1633(3) 0.34906(17) 0.0393(7) Uani 1 1 d . . . H21 H -0.0528 -0.2354 0.3725 0.047 Uiso 1 1 calc R . . C22 C 0.0330(3) -0.1606(3) 0.28627(16) 0.0347(7) Uani 1 1 d . . . H22 H 0.0501 -0.2317 0.2666 0.042 Uiso 1 1 calc R . . C23 C 0.0708(3) -0.0547(2) 0.25115(15) 0.0268(6) Uani 1 1 d . . . C24 C -0.0477(3) 0.1608(3) 0.37777(15) 0.0305(6) Uani 1 1 d . . . H24 H 0.0291 0.241 0.3663 0.037 Uiso 1 1 calc R . . C25 C -0.1829(3) 0.1533(3) 0.3470(2) 0.0457(8) Uani 1 1 d . . . H25C H -0.2597 0.0715 0.3532 0.069 Uiso 1 1 calc R . . H25B H -0.1761 0.1588 0.297 0.069 Uiso 1 1 calc R . . H25A H -0.2001 0.2248 0.371 0.069 Uiso 1 1 calc R . . C26 C -0.0485(4) 0.1759(4) 0.45770(18) 0.0496(9) Uani 1 1 d . . . H26C H 0.0368 0.1768 0.4775 0.074 Uiso 1 1 calc R . . H26B H -0.1295 0.1037 0.4708 0.074 Uiso 1 1 calc R . . H26A H -0.0535 0.2568 0.4759 0.074 Uiso 1 1 calc R . . C27 C 0.1322(3) -0.0597(3) 0.18034(15) 0.0328(6) Uani 1 1 d . . . H27 H 0.1407 0.0179 0.1606 0.039 Uiso 1 1 calc R . . C28 C 0.2766(4) -0.0556(3) 0.18505(18) 0.0441(8) Uani 1 1 d . . . H28C H 0.2739 -0.1256 0.2087 0.066 Uiso 1 1 calc R . . H28B H 0.3417 0.0271 0.2117 0.066 Uiso 1 1 calc R . . H28A H 0.3072 -0.0656 0.1378 0.066 Uiso 1 1 calc R . . C29 C 0.0341(4) -0.1784(3) 0.12913(18) 0.0456(8) Uani 1 1 d . . . H29C H 0.0299 -0.2563 0.1448 0.068 Uiso 1 1 calc R . . H29B H 0.069 -0.1735 0.0824 0.068 Uiso 1 1 calc R . . H29A H -0.0591 -0.1812 0.1275 0.068 Uiso 1 1 calc R . . C30 C 0.6895(3) 0.3736(3) 0.23537(15) 0.0304(6) Uani 1 1 d . . . H31B H 0.7314 0.4474 0.2098 0.036 Uiso 1 1 calc R . . H31A H 0.75 0.3281 0.2328 0.036 Uiso 1 1 calc R . . C31 C 0.6784(3) 0.4211(3) 0.31094(16) 0.0347(7) Uani 1 1 d . . . H32B H 0.6536 0.3499 0.3384 0.042 Uiso 1 1 calc R . . H32A H 0.7692 0.4906 0.3309 0.042 Uiso 1 1 calc R . . C32 C 0.5994(3) 0.5629(3) 0.37561(16) 0.0397(7) Uani 1 1 d . . . H33C H 0.6845 0.6398 0.3713 0.059 Uiso 1 1 calc R . . H33B H 0.6106 0.5284 0.4173 0.059 Uiso 1 1 calc R . . H33A H 0.5208 0.5856 0.3798 0.059 Uiso 1 1 calc R . . C33 C 0.5149(3) 0.2955(3) 0.13897(13) 0.0237(5) Uani 1 1 d . . . C34 C 0.3273(3) 0.2453(3) 0.05128(14) 0.0294(6) Uani 1 1 d . . . H35 H 0.393 0.2281 0.0193 0.035 Uiso 1 1 calc R . . C35 C 0.1855(3) 0.1309(3) 0.03691(15) 0.0387(7) Uani 1 1 d . . . H37C H 0.1206 0.1447 0.0691 0.058 Uiso 1 1 calc R . . H37B H 0.1938 0.0525 0.0439 0.058 Uiso 1 1 calc R . . H37A H 0.1506 0.1216 -0.0115 0.058 Uiso 1 1 calc R . . C36 C 0.3182(4) 0.3664(3) 0.03639(16) 0.0388(7) Uani 1 1 d . . . H36C H 0.411 0.4385 0.0438 0.058 Uiso 1 1 calc R . . H36B H 0.2556 0.3855 0.068 0.058 Uiso 1 1 calc R . . H36A H 0.2822 0.3531 -0.0122 0.058 Uiso 1 1 calc R . . C37 C 0.7193(3) 0.2961(3) 0.07652(15) 0.0361(7) Uani 1 1 d . . . H38 H 0.7677 0.3001 0.1218 0.043 Uiso 1 1 calc R . . C38 C 0.6520(4) 0.1568(4) 0.0407(2) 0.0581(10) Uani 1 1 d . . . H39C H 0.6051 0.1508 -0.0043 0.087 Uiso 1 1 calc R . . H39B H 0.5838 0.1044 0.0705 0.087 Uiso 1 1 calc R . . H39A H 0.7236 0.1255 0.0328 0.087 Uiso 1 1 calc R . . C39 C 0.8266(4) 0.3828(4) 0.03273(19) 0.0524(10) Uani 1 1 d . . . H40C H 0.8692 0.4711 0.0581 0.079 Uiso 1 1 calc R . . H40B H 0.7811 0.3808 -0.0118 0.079 Uiso 1 1 calc R . . H40A H 0.8986 0.3523 0.0237 0.079 Uiso 1 1 calc R . . C40 C 0.3305(4) 0.2563(4) 0.41776(17) 0.0456(8) Uani 1 1 d . . . H41B H 0.2375 0.2552 0.4123 0.055 Uiso 1 1 calc R . . H41A H 0.3989 0.3457 0.4351 0.055 Uiso 1 1 calc R . . C41 C 0.3292(6) 0.1710(4) 0.4675(2) 0.0642(12) Uani 1 1 d . . . H42B H 0.2338 0.1043 0.4705 0.077 Uiso 1 1 calc R . . H42A H 0.3668 0.2206 0.5148 0.077 Uiso 1 1 calc R . . C42 C 0.4225(5) 0.1110(4) 0.43664(19) 0.0611(11) Uani 1 1 d . . . H43B H 0.5213 0.166 0.4525 0.073 Uiso 1 1 calc R . . H43A H 0.3955 0.0247 0.4496 0.073 Uiso 1 1 calc R . . C43 C 0.3982(4) 0.1025(4) 0.36047(18) 0.0468(8) Uani 1 1 d . . . H44B H 0.482 0.1087 0.3362 0.056 Uiso 1 1 calc R . . H44A H 0.3191 0.02 0.341 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ca 0.0199(3) 0.0228(3) 0.0184(3) 0.00497(19) 0.00330(18) 0.0111(2) O1 0.0260(10) 0.0374(11) 0.0258(10) -0.0020(8) -0.0033(8) 0.0181(9) O3 0.0441(12) 0.0440(12) 0.0303(11) 0.0161(9) 0.0076(9) 0.0269(10) N1 0.0196(10) 0.0179(10) 0.0203(10) 0.0042(8) 0.0026(8) 0.0082(8) N2 0.0223(11) 0.0188(10) 0.0224(11) 0.0052(8) 0.0040(8) 0.0095(9) N3 0.0234(11) 0.0386(13) 0.0190(11) 0.0037(9) 0.0023(9) 0.0154(10) N4 0.0270(12) 0.0449(15) 0.0276(13) 0.0110(11) 0.0073(10) 0.0201(11) N5 0.0225(11) 0.0322(12) 0.0224(11) 0.0031(9) 0.0011(9) 0.0146(10) C1 0.0221(12) 0.0229(12) 0.0193(12) 0.0062(10) 0.0044(9) 0.0114(10) C2 0.0217(13) 0.0261(13) 0.0221(13) 0.0044(10) -0.0016(10) 0.0104(11) C3 0.0208(12) 0.0224(12) 0.0241(13) 0.0023(10) 0.0036(10) 0.0093(10) C4 0.0303(15) 0.0260(14) 0.0356(15) 0.0073(11) -0.0035(12) 0.0145(12) C5 0.0279(15) 0.0256(14) 0.0384(16) 0.0022(12) -0.0040(12) 0.0074(12) C6 0.0208(12) 0.0188(12) 0.0227(12) 0.0048(9) 0.0011(10) 0.0101(10) C7 0.0233(13) 0.0245(13) 0.0265(13) 0.0058(10) 0.0039(10) 0.0129(11) C8 0.0357(16) 0.0255(14) 0.0280(14) -0.0012(11) 0.0037(12) 0.0137(12) C9 0.0400(17) 0.0203(13) 0.0383(16) -0.0041(12) 0.0037(13) 0.0064(12) C10 0.0314(15) 0.0242(14) 0.0370(16) 0.0064(12) 0.0091(12) 0.0037(12) C11 0.0270(14) 0.0247(13) 0.0267(14) 0.0052(11) 0.0039(11) 0.0093(11) C12 0.0308(14) 0.0248(13) 0.0275(14) 0.0045(11) 0.0098(11) 0.0129(12) C13 0.0303(17) 0.060(2) 0.0433(19) 0.0145(16) 0.0098(14) 0.0165(16) C14 0.0449(19) 0.0464(18) 0.0327(16) 0.0148(14) 0.0118(14) 0.0193(15) C15 0.0379(16) 0.0271(14) 0.0278(15) 0.0062(11) 0.0108(12) 0.0051(12) C16 0.052(2) 0.049(2) 0.0436(19) 0.0170(15) 0.0215(16) 0.0290(17) C17 0.051(2) 0.077(3) 0.0327(17) 0.0224(17) 0.0144(15) 0.030(2) C18 0.0235(13) 0.0224(13) 0.0277(13) 0.0055(10) 0.0031(10) 0.0099(11) C19 0.0307(15) 0.0231(13) 0.0313(15) 0.0076(11) 0.0092(11) 0.0117(11) C20 0.0459(18) 0.0300(15) 0.0358(16) 0.0146(13) 0.0161(13) 0.0168(14) C21 0.0506(19) 0.0264(15) 0.0458(18) 0.0177(13) 0.0136(15) 0.0174(14) C22 0.0427(17) 0.0237(14) 0.0424(17) 0.0081(12) 0.0080(13) 0.0178(13) C23 0.0280(14) 0.0212(13) 0.0319(14) 0.0046(11) 0.0053(11) 0.0112(11) C24 0.0349(15) 0.0230(13) 0.0348(15) 0.0077(11) 0.0129(12) 0.0124(12) C25 0.0374(18) 0.0412(18) 0.061(2) 0.0017(16) 0.0086(16) 0.0214(15) C26 0.074(3) 0.050(2) 0.0375(18) 0.0099(15) 0.0221(17) 0.0375(19) C27 0.0424(17) 0.0242(14) 0.0340(15) 0.0037(11) 0.0093(13) 0.0166(13) C28 0.047(2) 0.0445(19) 0.0455(19) 0.0036(15) 0.0151(15) 0.0247(16) C29 0.058(2) 0.0384(18) 0.0393(18) -0.0011(14) 0.0043(15) 0.0224(16) C30 0.0226(14) 0.0399(16) 0.0312(15) 0.0012(12) -0.0010(11) 0.0173(12) C31 0.0259(14) 0.0472(18) 0.0341(16) -0.0024(13) -0.0055(12) 0.0215(14) C32 0.0401(18) 0.0490(19) 0.0321(16) -0.0077(14) -0.0053(13) 0.0257(15) C33 0.0242(13) 0.0278(13) 0.0219(13) 0.0039(10) 0.0044(10) 0.0138(11) C34 0.0282(14) 0.0449(17) 0.0174(13) 0.0038(11) 0.0032(10) 0.0182(13) C35 0.0383(17) 0.0462(18) 0.0239(14) 0.0007(13) -0.0048(12) 0.0122(14) C36 0.0436(18) 0.0484(19) 0.0264(15) 0.0093(13) 0.0013(13) 0.0208(15) C37 0.0299(15) 0.058(2) 0.0272(15) 0.0046(13) 0.0074(12) 0.0258(15) C38 0.062(2) 0.065(3) 0.058(2) -0.0031(19) 0.0077(19) 0.042(2) C39 0.0314(17) 0.088(3) 0.0387(18) 0.0151(18) 0.0151(14) 0.0244(18) C40 0.061(2) 0.052(2) 0.0373(18) 0.0113(15) 0.0126(16) 0.0357(18) C41 0.110(4) 0.080(3) 0.036(2) 0.0229(19) 0.023(2) 0.069(3) C42 0.107(4) 0.070(3) 0.0338(19) 0.0102(17) 0.002(2) 0.063(3) C43 0.066(2) 0.051(2) 0.0385(18) 0.0118(15) 0.0044(16) 0.0383(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ca N5 2.380(2) . ? Ca N3 2.408(2) . ? Ca N1 2.417(2) . ? Ca N2 2.432(2) . ? Ca O3 2.464(2) . ? Ca O1 2.5867(19) . ? O1 C32 1.422(3) . ? O1 C31 1.436(3) . ? O3 C40 1.434(4) . ? O3 C43 1.449(4) . ? N1 C1 1.323(3) . ? N1 C6 1.432(3) . ? N2 C3 1.327(3) . ? N2 C18 1.432(3) . ? N3 C33 1.332(3) . ? N3 C34 1.469(3) . ? N4 C33 1.408(3) . ? N4 C37 1.462(4) . ? N4 H4X 0.87(4) . ? N5 C33 1.338(3) . ? N5 C30 1.459(3) . ? C1 C2 1.414(4) . ? C1 C4 1.519(3) . ? C2 C3 1.407(4) . ? C2 H2 0.95 . ? C3 C5 1.519(4) . ? C4 H4C 0.98 . ? C4 H4B 0.98 . ? C4 H4A 0.98 . ? C5 H5C 0.98 . ? C5 H5B 0.98 . ? C5 H5A 0.98 . ? C6 C11 1.410(4) . ? C6 C7 1.413(4) . ? C7 C8 1.393(4) . ? C7 C12 1.519(4) . ? C8 C9 1.381(4) . ? C8 H8 0.95 . ? C9 C10 1.383(4) . ? C9 H9 0.95 . ? C10 C11 1.394(4) . ? C10 H10 0.95 . ? C11 C15 1.523(4) . ? C12 C13 1.515(4) . ? C12 C14 1.525(4) . ? C12 H12 1 . ? C13 H13C 0.98 . ? C13 H13B 0.98 . ? C13 H13A 0.98 . ? C14 H14C 0.98 . ? C14 H14B 0.98 . ? C14 H14A 0.98 . ? C15 C16 1.521(5) . ? C15 C17 1.533(5) . ? C15 H15 1 . ? C16 H16C 0.98 . ? C16 H16B 0.98 . ? C16 H16A 0.98 . ? C17 H17C 0.98 . ? C17 H17B 0.98 . ? C17 H17A 0.98 . ? C18 C23 1.410(4) . ? C18 C19 1.410(4) . ? C19 C20 1.395(4) . ? C19 C24 1.530(4) . ? C20 C21 1.385(4) . ? C20 H20 0.95 . ? C21 C22 1.382(4) . ? C21 H21 0.95 . ? C22 C23 1.401(4) . ? C22 H22 0.95 . ? C23 C27 1.526(4) . ? C24 C25 1.519(5) . ? C24 C26 1.532(4) . ? C24 H24 1 . ? C25 H25C 0.98 . ? C25 H25B 0.98 . ? C25 H25A 0.98 . ? C26 H26C 0.98 . ? C26 H26B 0.98 . ? C26 H26A 0.98 . ? C27 C28 1.519(5) . ? C27 C29 1.534(4) . ? C27 H27 1 . ? C28 H28C 0.98 . ? C28 H28B 0.98 . ? C28 H28A 0.98 . ? C29 H29C 0.98 . ? C29 H29B 0.98 . ? C29 H29A 0.98 . ? C30 C31 1.512(4) . ? C30 H31B 0.99 . ? C30 H31A 0.99 . ? C31 H32B 0.99 . ? C31 H32A 0.99 . ? C32 H33C 0.98 . ? C32 H33B 0.98 . ? C32 H33A 0.98 . ? C34 C36 1.520(4) . ? C34 C35 1.520(4) . ? C34 H35 1 . ? C35 H37C 0.98 . ? C35 H37B 0.98 . ? C35 H37A 0.98 . ? C36 H36C 0.98 . ? C36 H36B 0.98 . ? C36 H36A 0.98 . ? C37 C38 1.518(5) . ? C37 C39 1.521(5) . ? C37 H38 1 . ? C38 H39C 0.98 . ? C38 H39B 0.98 . ? C38 H39A 0.98 . ? C39 H40C 0.98 . ? C39 H40B 0.98 . ? C39 H40A 0.98 . ? C40 C41 1.475(5) . ? C40 H41B 0.99 . ? C40 H41A 0.99 . ? C41 C42 1.519(5) . ? C41 H42B 0.99 . ? C41 H42A 0.99 . ? C42 C43 1.478(5) . ? C42 H43B 0.99 . ? C42 H43A 0.99 . ? C43 H44B 0.99 . ? C43 H44A 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ca N3 56.59(7) . . ? N5 Ca N1 133.68(8) . . ? N3 Ca N1 102.65(8) . . ? N5 Ca N2 141.92(8) . . ? N3 Ca N2 103.26(8) . . ? N1 Ca N2 78.69(7) . . ? N5 Ca O3 92.08(7) . . ? N3 Ca O3 137.06(8) . . ? N1 Ca O3 120.17(7) . . ? N2 Ca O3 83.39(7) . . ? N5 Ca O1 66.59(7) . . ? N3 Ca O1 111.10(7) . . ? N1 Ca O1 89.38(7) . . ? N2 Ca O1 145.35(7) . . ? O3 Ca O1 74.70(7) . . ? C32 O1 C31 111.8(2) . . ? C32 O1 Ca 132.36(17) . . ? C31 O1 Ca 109.48(16) . . ? C40 O3 C43 108.8(2) . . ? C40 O3 Ca 119.96(17) . . ? C43 O3 Ca 130.89(18) . . ? C1 N1 C6 118.9(2) . . ? C1 N1 Ca 116.10(16) . . ? C6 N1 Ca 123.51(15) . . ? C3 N2 C18 119.6(2) . . ? C3 N2 Ca 114.08(16) . . ? C18 N2 Ca 122.19(16) . . ? C33 N3 C34 120.3(2) . . ? C33 N3 Ca 90.21(15) . . ? C34 N3 Ca 147.43(17) . . ? C33 N4 C37 120.6(2) . . ? C33 N4 H4X 115(3) . . ? C37 N4 H4X 109(2) . . ? C33 N5 C30 119.1(2) . . ? C33 N5 Ca 91.27(15) . . ? C30 N5 Ca 122.02(17) . . ? N1 C1 C2 124.8(2) . . ? N1 C1 C4 120.9(2) . . ? C2 C1 C4 114.2(2) . . ? C3 C2 C1 131.3(2) . . ? C3 C2 H2 114.4 . . ? C1 C2 H2 114.4 . . ? N2 C3 C2 124.2(2) . . ? N2 C3 C5 120.7(2) . . ? C2 C3 C5 115.1(2) . . ? C1 C4 H4C 109.5 . . ? C1 C4 H4B 109.5 . . ? H4C C4 H4B 109.5 . . ? C1 C4 H4A 109.5 . . ? H4C C4 H4A 109.5 . . ? H4B C4 H4A 109.5 . . ? C3 C5 H5C 109.5 . . ? C3 C5 H5B 109.5 . . ? H5C C5 H5B 109.5 . . ? C3 C5 H5A 109.5 . . ? H5C C5 H5A 109.5 . . ? H5B C5 H5A 109.5 . . ? C11 C6 C7 119.9(2) . . ? C11 C6 N1 122.0(2) . . ? C7 C6 N1 118.0(2) . . ? C8 C7 C6 119.2(2) . . ? C8 C7 C12 120.4(2) . . ? C6 C7 C12 120.5(2) . . ? C9 C8 C7 120.9(3) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 119.8(3) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C11 121.3(3) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C6 118.7(2) . . ? C10 C11 C15 118.7(2) . . ? C6 C11 C15 122.5(2) . . ? C13 C12 C7 111.7(2) . . ? C13 C12 C14 110.3(2) . . ? C7 C12 C14 112.6(2) . . ? C13 C12 H12 107.3 . . ? C7 C12 H12 107.3 . . ? C14 C12 H12 107.3 . . ? C12 C13 H13C 109.5 . . ? C12 C13 H13B 109.5 . . ? H13C C13 H13B 109.5 . . ? C12 C13 H13A 109.5 . . ? H13C C13 H13A 109.5 . . ? H13B C13 H13A 109.5 . . ? C12 C14 H14C 109.5 . . ? C12 C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? C12 C14 H14A 109.5 . . ? H14C C14 H14A 109.5 . . ? H14B C14 H14A 109.5 . . ? C16 C15 C11 111.8(3) . . ? C16 C15 C17 109.2(3) . . ? C11 C15 C17 111.5(3) . . ? C16 C15 H15 108.1 . . ? C11 C15 H15 108.1 . . ? C17 C15 H15 108.1 . . ? C15 C16 H16C 109.5 . . ? C15 C16 H16B 109.5 . . ? H16C C16 H16B 109.5 . . ? C15 C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? C15 C17 H17C 109.5 . . ? C15 C17 H17B 109.5 . . ? H17C C17 H17B 109.5 . . ? C15 C17 H17A 109.5 . . ? H17C C17 H17A 109.5 . . ? H17B C17 H17A 109.5 . . ? C23 C18 C19 120.4(2) . . ? C23 C18 N2 120.8(2) . . ? C19 C18 N2 118.6(2) . . ? C20 C19 C18 118.7(3) . . ? C20 C19 C24 120.5(2) . . ? C18 C19 C24 120.8(2) . . ? C21 C20 C19 121.4(3) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C22 C21 C20 119.7(3) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 121.1(3) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 118.7(3) . . ? C22 C23 C27 118.8(2) . . ? C18 C23 C27 122.5(2) . . ? C25 C24 C19 112.3(3) . . ? C25 C24 C26 109.4(3) . . ? C19 C24 C26 113.5(2) . . ? C25 C24 H24 107.1 . . ? C19 C24 H24 107.1 . . ? C26 C24 H24 107.1 . . ? C24 C25 H25C 109.5 . . ? C24 C25 H25B 109.5 . . ? H25C C25 H25B 109.5 . . ? C24 C25 H25A 109.5 . . ? H25C C25 H25A 109.5 . . ? H25B C25 H25A 109.5 . . ? C24 C26 H26C 109.5 . . ? C24 C26 H26B 109.5 . . ? H26C C26 H26B 109.5 . . ? C24 C26 H26A 109.5 . . ? H26C C26 H26A 109.5 . . ? H26B C26 H26A 109.5 . . ? C28 C27 C23 113.4(3) . . ? C28 C27 C29 110.2(3) . . ? C23 C27 C29 110.8(3) . . ? C28 C27 H27 107.4 . . ? C23 C27 H27 107.4 . . ? C29 C27 H27 107.4 . . ? C27 C28 H28C 109.5 . . ? C27 C28 H28B 109.5 . . ? H28C C28 H28B 109.5 . . ? C27 C28 H28A 109.5 . . ? H28C C28 H28A 109.5 . . ? H28B C28 H28A 109.5 . . ? C27 C29 H29C 109.5 . . ? C27 C29 H29B 109.5 . . ? H29C C29 H29B 109.5 . . ? C27 C29 H29A 109.5 . . ? H29C C29 H29A 109.5 . . ? H29B C29 H29A 109.5 . . ? N5 C30 C31 109.1(2) . . ? N5 C30 H31B 109.9 . . ? C31 C30 H31B 109.9 . . ? N5 C30 H31A 109.9 . . ? C31 C30 H31A 109.9 . . ? H31B C30 H31A 108.3 . . ? O1 C31 C30 109.7(2) . . ? O1 C31 H32B 109.7 . . ? C30 C31 H32B 109.7 . . ? O1 C31 H32A 109.7 . . ? C30 C31 H32A 109.7 . . ? H32B C31 H32A 108.2 . . ? O1 C32 H33C 109.5 . . ? O1 C32 H33B 109.5 . . ? H33C C32 H33B 109.5 . . ? O1 C32 H33A 109.5 . . ? H33C C32 H33A 109.5 . . ? H33B C32 H33A 109.5 . . ? N3 C33 N5 116.5(2) . . ? N3 C33 N4 122.8(2) . . ? N5 C33 N4 120.6(2) . . ? N3 C34 C36 111.5(2) . . ? N3 C34 C35 109.8(2) . . ? C36 C34 C35 110.2(3) . . ? N3 C34 H35 108.4 . . ? C36 C34 H35 108.4 . . ? C35 C34 H35 108.4 . . ? C34 C35 H37C 109.5 . . ? C34 C35 H37B 109.5 . . ? H37C C35 H37B 109.5 . . ? C34 C35 H37A 109.5 . . ? H37C C35 H37A 109.5 . . ? H37B C35 H37A 109.5 . . ? C34 C36 H36C 109.5 . . ? C34 C36 H36B 109.5 . . ? H36C C36 H36B 109.5 . . ? C34 C36 H36A 109.5 . . ? H36C C36 H36A 109.5 . . ? H36B C36 H36A 109.5 . . ? N4 C37 C38 112.2(3) . . ? N4 C37 C39 108.2(3) . . ? C38 C37 C39 112.0(3) . . ? N4 C37 H38 108.1 . . ? C38 C37 H38 108.1 . . ? C39 C37 H38 108.1 . . ? C37 C38 H39C 109.5 . . ? C37 C38 H39B 109.5 . . ? H39C C38 H39B 109.5 . . ? C37 C38 H39A 109.5 . . ? H39C C38 H39A 109.5 . . ? H39B C38 H39A 109.5 . . ? C37 C39 H40C 109.5 . . ? C37 C39 H40B 109.5 . . ? H40C C39 H40B 109.5 . . ? C37 C39 H40A 109.5 . . ? H40C C39 H40A 109.5 . . ? H40B C39 H40A 109.5 . . ? O3 C40 C41 107.6(3) . . ? O3 C40 H41B 110.2 . . ? C41 C40 H41B 110.2 . . ? O3 C40 H41A 110.2 . . ? C41 C40 H41A 110.2 . . ? H41B C40 H41A 108.5 . . ? C40 C41 C42 103.6(3) . . ? C40 C41 H42B 111 . . ? C42 C41 H42B 111 . . ? C40 C41 H42A 111 . . ? C42 C41 H42A 111 . . ? H42B C41 H42A 109 . . ? C43 C42 C41 103.1(3) . . ? C43 C42 H43B 111.1 . . ? C41 C42 H43B 111.1 . . ? C43 C42 H43A 111.1 . . ? C41 C42 H43A 111.1 . . ? H43B C42 H43A 109.1 . . ? O3 C43 C42 105.9(3) . . ? O3 C43 H44B 110.6 . . ? C42 C43 H44B 110.6 . . ? O3 C43 H44A 110.6 . . ? C42 C43 H44A 110.6 . . ? H44B C43 H44A 108.7 . . ? #===END